WO2018150952A1 - Soft magnetic powder, dust magnetic core, magnetic part, and method for producing dust magnetic core - Google Patents

Soft magnetic powder, dust magnetic core, magnetic part, and method for producing dust magnetic core Download PDF

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Publication number
WO2018150952A1
WO2018150952A1 PCT/JP2018/004021 JP2018004021W WO2018150952A1 WO 2018150952 A1 WO2018150952 A1 WO 2018150952A1 JP 2018004021 W JP2018004021 W JP 2018004021W WO 2018150952 A1 WO2018150952 A1 WO 2018150952A1
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Prior art keywords
soft magnetic
magnetic powder
powder
core
mass
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PCT/JP2018/004021
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French (fr)
Japanese (ja)
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浦田　顕理
美帆 千葉
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株式会社トーキン
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Priority to CN201880001453.2A priority Critical patent/CN108883465B/en
Priority to KR1020187026801A priority patent/KR101932422B1/en
Priority to US16/089,334 priority patent/US10847291B2/en
Priority to EP18754111.5A priority patent/EP3549696B1/en
Publication of WO2018150952A1 publication Critical patent/WO2018150952A1/en

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Definitions

  • the present invention relates to a soft magnetic powder suitable for use in magnetic parts such as a dust core.
  • Patent Document 1 discloses a soft magnetic alloy made of Fe, Si, B, and Cu.
  • the soft magnetic alloy of Patent Document 1 is manufactured as a ribbon by quenching a molten alloy having a predetermined element composition by a roll quenching method.
  • Patent Document 2 discloses as Example 5 a soft magnetic powder having an elemental composition containing 0.09% by mass of Cu in Fe bal Si 10 B 11 P 5 Cr 0.5 .
  • the water atomization method is adopted as the rapid cooling method.
  • a soft magnetic alloy used for a magnetic part such as a dust core powder is required from the viewpoint of ease of forming into a desired shape.
  • a pulverization step is separately required, and the process becomes complicated, and at the same time, the production of the spherical powder is difficult and the formability is poor.
  • the soft magnetic powder can be obtained directly from the molten alloy, a simplified process There is an advantage that soft magnetic powder can be produced.
  • the soft magnetic alloy of Patent Document 1 does not contain Cr, which is an element imparting rust prevention, rust may be generated in the powder when treated with water, and the produced soft magnetic alloy Lack of powder reliability.
  • the soft magnetic powder of Example 5 of Patent Document 2 contains Cr, which is an element that imparts rust prevention properties, but soft magnetic properties deteriorate because it contains a large amount of Si and B. there is a possibility.
  • an object of the present invention is to provide a soft magnetic powder that is highly compatible with rust prevention and soft magnetic properties.
  • a soft magnetic powder represented by the composition formula Fe a Si b B c P d Cr e M f excluding inevitable impurities, M is one or more elements selected from V, Mn, Co, Ni, Cu, Zn, Soft magnetic powder with 0 at% ⁇ b ⁇ 6 at%, 4 at% ⁇ c ⁇ 10 at%, 5 at% ⁇ d ⁇ 12 at%, 0 at% ⁇ e, 0.4 at% ⁇ f ⁇ 6 at%, and a + b + c + d + e + f 100 at% I will provide a.
  • the soft magnetic powder according to the present invention contains a predetermined range of Fe, Si, B, P, Cr, and M (one or more elements selected from V, Mn, Co, Ni, Cu, and Zn). Is formed on the surface of the powder, and an amorphous phase can be contained in a high proportion. Thereby, in the soft magnetic powder of this invention, rust prevention property and soft magnetic characteristic are highly compatible. In addition, since the soft magnetic powder of the present invention has rust prevention properties, in the manufacturing process of the soft magnetic powder of the present invention, a rapid cooling method using a coolant such as water having excellent mass productivity and high cooling performance is used. Can be adopted.
  • Soft magnetic powder according to the present embodiment is expressed by a composition formula except inevitable impurities Fe a Si b B c P d Cr e M f.
  • the soft magnetic powder of this embodiment can be used as a direct material for producing various magnetic parts, dust cores, and inductor cores.
  • the soft magnetic powder of the present embodiment can be manufactured by a manufacturing method such as an atomizing method.
  • the soft magnetic powder thus produced has an amorphous phase as the main phase.
  • the soft magnetic powder of the present invention preferably contains nanocrystals.
  • the soft magnetic powder containing nanocrystals is obtained by subjecting the soft magnetic powder to heat treatment under predetermined heat treatment conditions to precipitate bccFe ( ⁇ Fe) nanocrystals as described later.
  • crystallization start temperature Tx1
  • second crystallization start temperature Tx2
  • ⁇ T Tx2 ⁇ Tx1
  • the first crystallization start temperature (Tx1) is an exothermic peak of ⁇ Fe nanocrystal precipitation
  • the second crystallization start temperature (Tx2) is an exothermic peak of precipitation of compounds such as FeB and FeP.
  • DSC differential scanning calorimetry
  • ⁇ Fe nanocrystals In order to precipitate ⁇ Fe nanocrystals in the soft magnetic powder, it is desirable to perform heat treatment at a temperature equal to or lower than the second crystallization start temperature (Tx2) so as to suppress the precipitation of the compound phase.
  • Tx2 the second crystallization start temperature
  • ⁇ T when ⁇ T is large, heat treatment under a predetermined heat treatment condition is facilitated. Therefore, only ⁇ Fe nanocrystals can be precipitated by heat treatment to obtain a soft magnetic powder having good soft magnetic properties. That is, by adjusting the elemental composition of the soft magnetic powder so that ⁇ T is increased and heat-treating, the ⁇ Fe nanocrystal structure contained in the soft magnetic powder is stabilized, and the pressure provided with the soft magnetic powder containing the ⁇ Fe nanocrystal is stabilized. The core loss of the magnetic core of the powder magnetic core or the inductor is also reduced.
  • composition range of the soft magnetic powder according to the present embodiment will be described in more detail.
  • the Fe element is a main element and an essential element responsible for magnetism.
  • the ratio of Fe is large.
  • the proportion of Fe is preferably 78 at% or more, and preferably 85 at% or less.
  • the ratio of Fe is 78 at% or more, ⁇ T can be increased in addition to the above effects.
  • it is more preferably 79 at% or more, and further preferably 80.5 at% or more.
  • the Fe ratio is preferably 83.5 at% or less.
  • the Si element is an element responsible for forming an amorphous phase, and contributes to the stabilization of the nanocrystal in the nanocrystallization.
  • the Si ratio needs to be 6 at% or less (including zero) in order to reduce the core loss of the dust core and the inductor core.
  • the proportion of Si exceeds 6 at%, the amount of Si is excessive, so that the amorphous forming ability is lowered, and a soft magnetic powder having an amorphous phase of 90% or more cannot be obtained.
  • the proportion of Si is 0.1 at% or more It is more preferable.
  • the ratio of Si is more preferably 2 at% or more in order to increase ⁇ T.
  • the B element is an essential element responsible for forming an amorphous phase.
  • the ratio of B needs to be 4 at% or more and 10 at% or less in order to reduce the core loss of the powder magnetic core or the magnetic core of the inductor by setting the amorphous phase of the soft magnetic powder to 90% or more. If the ratio of B exceeds 10 at%, the melting point of the molten alloy increases rapidly, which is not preferable for production, and the amorphous forming ability is also lowered. On the other hand, when the ratio of B becomes smaller than 4 at%, the balance of Si, B, and P, which are metalloid elements, is deteriorated and the amorphous forming ability is lowered.
  • the P element is an essential element for forming an amorphous phase.
  • the proportion of P according to the present embodiment is not less than 5 at% and not more than 12 at%.
  • the proportion of P is 5 at% or more, the amorphous forming ability is improved, the amorphous phase is increased, and stable soft magnetic characteristics can be obtained.
  • the proportion of P exceeds 12 at%, the balance of the metalloid elements Si, B, and P is deteriorated, the amorphous forming ability is lowered, and at the same time, the saturation magnetic flux density Bs is significantly lowered.
  • the ratio of P it is preferable to set the ratio of P to 10 at% or less because a decrease in saturation magnetic flux density Bs can be suppressed. Furthermore, it is more preferable that the ratio of P is 8 at% or less because a uniform nanostructure can be easily obtained after heat treatment and good soft magnetic properties can be obtained. On the other hand, when the ratio of P exceeds 5 at%, it is preferable because amorphous forming ability is improved and more stable soft magnetic characteristics can be obtained. In addition, when the ratio of P exceeds 6 at%, the corrosion resistance is remarkably improved, and when it exceeds 8 at%, the soft magnetic powder at the time of atomization progresses to spheroidize, so that the filling rate is improved and the corrosion resistance is further increased. It is more preferable because a uniform nanostructure can be easily obtained.
  • Cr element is an essential element contributing to rust prevention.
  • the proportion of Cr according to the present embodiment is greater than 0 at%. Specifically, when the proportion of Cr is greater than 0 at%, an oxide film is formed on the surface of the soft magnetic powder, so that rust prevention is imparted and the proportion of the amorphous phase is improved. Since an oxide film is formed on the surface of the soft magnetic powder, rust occurs on the surface of the soft magnetic powder even when the soft magnetic powder is manufactured by a cooling method using water. There is no.
  • the Cr ratio is preferably 3 at% or less in order to obtain a high saturation magnetic flux density Bs in the soft magnetic powder, and more preferably 1.8 at% or less in consideration of reduction of core loss.
  • the Cr ratio is preferably 1.5 at% or less in order to obtain a high saturation magnetic flux density Bs, and more preferably 1.0 at% or less in order to obtain a higher saturation magnetic flux density Bs.
  • the ratio of Cr is preferably 0.1 at% or more, and more preferably 0.5 at% or more in order to improve rust prevention.
  • M element is an essential element in the soft magnetic powder according to the present embodiment.
  • the proportion of M according to the present embodiment is 0.4 at% or more and less than 6 at%.
  • the corrosion resistance is remarkably improved.
  • the proportion of M needs to be 0.4 at% or more in order to prevent the coarsening of the nanocrystals in the soft magnetic powder and obtain a desired core loss in the dust core.
  • M element satisfies the above-described conditions, the rust prevention property and the amorphous forming ability are further improved in the soft magnetic powder.
  • the ratio of Cu is less than 0.7 at%, a powder having a high ratio of the amorphous phase is obtained, and preferably 0.65 at% or less.
  • the precipitation amount of ⁇ Fe nanocrystals is increased and a uniform nanostructure is easily obtained, and if it is 0.5 at% or more, corrosion resistance is remarkably improved and ⁇ Fe This is more preferable because the amount of deposited nanocrystals is further increased and soft magnetic properties are improved.
  • the Cr ratio is e (at%).
  • the ratio of Cu is preferably (0.2e ⁇ 0.1) at% or more and (2e + 0.5) at% or less.
  • the ratio of P is preferably (6-2e) at% or more and (21-5e) at% or less.
  • the soft magnetic powder according to the present embodiment 3 at% or less of Fe, Nb, Zr, Hf, Mo, Ta, W, Ag, Au, Pd, K, Ca, Mg, Sn, Ti, Al, S, C
  • One obtained by substituting one or more elements selected from O, N, Y and rare earth elements is preferable. By including such an element, uniform nanocrystallization after the heat treatment is facilitated.
  • the soft magnetic powder may contain these trace elements in various contents. These trace elements affect the soft magnetic properties of the soft magnetic powder produced. Therefore, in order to obtain good soft magnetic characteristics in the produced soft magnetic powder, it is necessary to control the contents of these trace elements contained in the soft magnetic powder.
  • Al is a trace element mixed in the soft magnetic powder produced by using industrial raw materials such as Fe—P and Fe—B.
  • the content of Al is preferably 0.05% by mass or less in order to avoid a decrease in the ratio of amorphous, and further improvement of the ratio of amorphous and suppression of influence on soft magnetic properties are suppressed. Therefore, it is more preferable to set it as 0.005 mass% or less.
  • Ti is a trace element mixed in the soft magnetic powder produced by using industrial raw materials such as Fe-P and Fe-B. Incorporation of Ti into the soft magnetic powder causes a decrease in the amorphous ratio and soft magnetic properties. Therefore, the Ti content is preferably 0.05% by mass or less in order to avoid a decrease in the amorphous ratio, which further improves the amorphous ratio and suppresses the influence on the soft magnetic properties. Therefore, it is more preferable to set it as 0.005 mass% or less.
  • S is a trace element mixed in the soft magnetic powder produced by using industrial raw materials such as Fe-P and Fe-B.
  • the addition of a small amount of S has the effect of promoting the spheroidization of the soft magnetic powder.
  • the S content is preferably 0.5% by mass or less, and more preferably 0.05% by mass or less in order to avoid a decrease in soft magnetic properties.
  • N is a trace element derived from industrial raw materials or mixed into the soft magnetic powder from the air during atomization or heat treatment. Incorporation of N into the soft magnetic powder leads to a decrease in the amorphous ratio of the soft magnetic powder, a decrease in filling rate when the soft magnetic powder is formed, and a decrease in soft magnetic characteristics. Therefore, the N content is preferably 0.01% by mass or less, and more preferably 0.002% by mass or less, in order to suppress a decrease in the amorphous ratio and soft magnetic properties.
  • O is a trace element derived from industrial raw materials, or mixed in the soft magnetic powder from the air during atomization or drying. Incorporation of ⁇ into the soft magnetic powder leads to a decrease in the amorphous ratio of the soft magnetic powder, a decrease in the filling rate when the soft magnetic powder is formed, and a decrease in the soft magnetic properties. Therefore, the content of O is preferably set to 1.0% by mass or less in order to suppress a decrease in the ratio of amorphous, and a decrease in filling rate when soft magnetic powder is molded or a soft magnetic property. In order to suppress the decrease in the amount, it is more preferably set to 0.3% by mass or less.
  • the oxide film containing Cr is formed on the surface of the soft magnetic powder, a small amount of O is intentionally contained in the soft magnetic powder.
  • the insulating property between the soft magnetic powders may be improved by forming an insulating coating on the surface of the soft magnetic powder with resin or ceramic.
  • the content of O including the insulating coating may exceed 1.0% by mass.
  • the soft magnetic powder according to the present embodiment can be produced by various manufacturing methods.
  • the soft magnetic powder may be produced by an atomizing method such as a water atomizing method or a gas atomizing method.
  • the soft magnetic powder of this Embodiment contains Cr which provides rust prevention property, even if it produces with the cooling method using water, it does not produce rust on the surface of powder.
  • the powder preparation process by the atomizing method first, raw materials are prepared. Next, the raw materials are weighed so as to have a predetermined composition and melted to produce a molten alloy. At this time, since the soft magnetic powder of the present embodiment has a low melting point, power consumption for dissolution can be reduced. Next, the molten alloy is discharged from the nozzle and divided into alloy droplets using high-pressure gas or water, thereby producing a fine soft magnetic powder.
  • the gas used for cutting may be an inert gas such as argon or nitrogen.
  • the alloy droplets immediately after the division may be brought into contact with a cooling liquid or solid to be rapidly cooled, or the alloy droplets may be redivided and further refined.
  • a liquid for cooling for example, water or oil may be used.
  • a solid for cooling, for example, a rotating copper roll or a rotating aluminum plate may be used.
  • the cooling liquid or solid is not limited to this, and various materials can be used.
  • the soft magnetic powder of this Embodiment contains Cr which provides rust prevention property, the cooling method using the water excellent in mass-productivity is employable.
  • the powder shape and particle size of the soft magnetic powder can be adjusted by changing the production conditions.
  • the viscosity of the molten alloy is low, it is easy to produce a soft magnetic powder into a spherical shape.
  • the average particle size of the soft magnetic powder of the present embodiment is preferably 200 ⁇ m or less, and more preferably 100 ⁇ m or less in order to improve the degree of amorphization.
  • the maximum particle diameter of the soft magnetic powder is preferably 200 ⁇ m or less.
  • the soft magnetic powder of the present embodiment preferably contains 90% or more of an amorphous phase.
  • the soft magnetic powder of the present embodiment has excellent soft magnetic properties.
  • the soft magnetic powder of the present embodiment has a tap density of 3.5 g / cm 3 or more.
  • the particle size of the soft magnetic powder can be evaluated by a laser particle size distribution meter.
  • the average particle size of the soft magnetic powder can be calculated from the evaluated particle size. From the peak position of the X-ray diffraction result of the soft magnetic powder, the precipitated phase such as ⁇ Fe (-Si) phase and compound phase can be identified.
  • the tap density test method follows the standard JIS Z2512 (metal powder-tap density measurement method).
  • the average particle diameter of the ⁇ Fe nanocrystals precipitated in the soft magnetic powder by the heat treatment exceeds 50 nm, the magnetocrystalline anisotropy increases and the soft magnetic properties deteriorate. Further, when the average particle diameter of the ⁇ Fe nanocrystal exceeds 40 nm, the soft magnetic characteristics are somewhat deteriorated. Accordingly, the average particle diameter of the ⁇ Fe nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
  • the crystallinity of the ⁇ Fe nanocrystals precipitated in the soft magnetic powder by the heat treatment is 35% or more, the saturation magnetic flux density Bs is improved to 1.6 T or more. Therefore, the crystallinity of ⁇ Fe nanocrystals is preferably 35% or more. Further, the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals precipitated in the soft magnetic powder by the heat treatment is preferably 7% or less, preferably 5% or less, from the viewpoint of suppressing the decrease in soft magnetic properties. Is more preferable, and 3% or less is still more preferable.
  • the average particle diameter and crystallinity of the above-mentioned ⁇ Fe nanocrystals, and the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals were measured by X-ray diffraction (XRD: X-ray diffraction). It can be calculated by analyzing by the method (Whole-powder-pattern decomposition method).
  • the saturation magnetic flux density Bs can be calculated from the saturation magnetization measured using a vibrating sample magnetometer (VSM) and the density.
  • a powder magnetic core can be manufactured using the soft magnetic powder produced from the above-mentioned powder production process.
  • the powder magnetic core can be manufactured by forming a soft magnetic powder into a predetermined shape and then performing heat treatment under predetermined heat treatment conditions.
  • magnetic parts such as a transformer, an inductor, a motor, and a generator, can be manufactured using this powder magnetic core.
  • the manufacturing method of the powder magnetic core of this Embodiment using soft magnetic powder is demonstrated.
  • the method for producing a dust core according to the present embodiment includes a step of producing a mixture of the soft magnetic powder and a binder according to the present embodiment, a step of producing a molded body by press molding the mixture, And a step of heat-treating the molded body.
  • the soft magnetic powder of the present embodiment is mixed with a binder having good insulating properties such as a resin to obtain a mixture (granulated powder).
  • a binder having good insulating properties such as a resin
  • a resin for example, silicone, epoxy, phenol, melamine, polyurethane, polyimide, or polyamideimide may be used.
  • phosphate, borate, chromate, oxide (silica, alumina, magnesia, etc.), inorganic polymer (polysilane) instead of or together with resin may be used as the binder.
  • Polygermane, polystannane, polysiloxane, polysilsesquioxane, polysilazane, polyborazirene, polyphosphazene, and the like may be used as the binder.
  • a plurality of binders may be used in combination, and a coating having a multilayer structure of two layers or more may be formed by different binders.
  • the amount of the binder is preferably about 0.1 to 10% by mass, and is preferably about 0.3 to 6% by mass in consideration of insulation and filling rate.
  • the amount of the binder may be appropriately determined in consideration of the powder particle size, application frequency, usage, and the like.
  • the molded powder is obtained by pressure molding the granulated powder using a mold.
  • the granulated powder Fe, FeSi, FeSiCr, FeSiAl, FeNi, softer than the soft magnetic powder according to the present embodiment, in order to improve the filling rate and suppress heat generation in nanocrystallization.
  • One or more kinds of powders such as carbonyl iron powder may be mixed.
  • any soft magnetic powder having a particle diameter different from that of the soft magnetic powder according to the present embodiment may be mixed.
  • the mixing ratio of the powder to the soft magnetic powder according to the present embodiment is preferably 75% by mass or less.
  • the molded body is subjected to heat treatment under predetermined heat treatment conditions.
  • This heat treatment is the same as the heat treatment for the soft magnetic powder described above, and it is necessary to perform the heat treatment at or below the second crystallization start temperature (Tx2).
  • This heat treatment is preferably performed at a temperature of 300 ° C. or higher in an inert atmosphere such as argon or nitrogen.
  • an inert atmosphere such as argon or nitrogen.
  • it may be partially heat-treated in an oxidizing atmosphere.
  • you may heat-process partially in a reducing atmosphere.
  • the average particle diameter of the ⁇ Fe nanocrystals precipitated in the soft magnetic powder constituting the dust core by the heat treatment described above exceeds 50 nm, the magnetocrystalline anisotropy increases and the soft magnetic properties deteriorate. Further, when the average particle diameter of the ⁇ Fe nanocrystal exceeds 40 nm, the soft magnetic characteristics are somewhat deteriorated. Accordingly, the average particle diameter of the ⁇ Fe nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
  • the crystallinity of the ⁇ Fe nanocrystals precipitated in the soft magnetic powder constituting the powder magnetic core by the heat treatment described above is 35% or more, the saturation magnetic flux density of the powder magnetic core is improved and the magnetostriction can be reduced. Further, the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals precipitated in the soft magnetic powder constituting the powder magnetic core by the above heat treatment is 7% from the viewpoint of reducing the core loss of the powder magnetic core. The following is preferable, 5% or less is more preferable, and 3% or less is still more preferable.
  • the average particle diameter and crystallinity of the above-mentioned ⁇ Fe nanocrystals, and the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals were measured by X-ray diffraction (XRD: X-ray diffraction). It can be calculated by analyzing by the method (Whole-powder-pattern decomposition method).
  • the dust core in the present embodiment is manufactured using soft magnetic powder that has not been heat-treated as a raw material.
  • the present invention is not limited to this, and soft magnetism in which ⁇ Fe nanocrystals are deposited in advance by heat treatment. You may manufacture a powder magnetic core from powder.
  • a dust core can be manufactured by granulating and press-molding similarly to the manufacturing process of the above-mentioned dust core.
  • the magnetic core of the inductor can also be manufactured using the soft magnetic powder produced from the above-mentioned powder production process.
  • a method of manufacturing the inductor magnetic core according to the present embodiment using soft magnetic powder will be described.
  • the inductor magnetic core manufacturing method includes a step of manufacturing the mixture of the soft magnetic powder and the binder according to the present embodiment, and press-molding the mixture and the coil together to form a molded body.
  • the manufacturing process and the process of heat-processing this molded object are provided.
  • the process for producing the mixture of the soft magnetic powder and the binder according to the present embodiment is the same as the above-described method for producing a dust core, and detailed description thereof is omitted.
  • the mixture (granulated powder) is put into the mold and the mixture (granulated powder) ) And the coil are integrally pressure-molded to obtain a molded body.
  • the mixture (granulated powder) and the coil are integrally pressure-molded, in order to improve the filling rate and suppress heat generation in nanocrystallization, Fe that is softer than the soft magnetic powder according to the present embodiment, One or more kinds of powders such as FeSi, FeSiCr, FeSiAl, FeNi, and carbonyl iron powder may be mixed.
  • any soft magnetic powder having a particle diameter different from that of the soft magnetic powder according to the present embodiment may be mixed.
  • the mixing ratio of the powder to the soft magnetic powder according to the present embodiment is preferably 75% by mass or less.
  • the process of heat-treating the molded body is also the same as the above-described method for manufacturing a dust core, and detailed description thereof is omitted.
  • the average particle diameter of the ⁇ Fe nanocrystals precipitated in the soft magnetic powder constituting the magnetic core of the inductor by the above heat treatment exceeds 50 nm, the magnetocrystalline anisotropy increases and the soft magnetic properties deteriorate. Further, when the average particle diameter of the ⁇ Fe nanocrystal exceeds 40 nm, the soft magnetic characteristics are somewhat deteriorated. Accordingly, the average particle diameter of the ⁇ Fe nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
  • the crystallinity of the ⁇ Fe nanocrystals deposited in the soft magnetic powder constituting the magnetic core of the inductor by the above heat treatment is 35% or more, the saturation magnetic flux density of the powder magnetic core is improved and the magnetostriction can be reduced. Further, the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals precipitated in the soft magnetic powder constituting the magnetic core of the inductor by the heat treatment described above is 7% from the viewpoint of reducing the core loss of the magnetic core of the inductor. The following is preferable, 5% or less is more preferable, and 3% or less is still more preferable.
  • the average particle size and crystallinity of the ⁇ Fe nanocrystals and the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals can be measured in the same manner as in the case of the above-described dust core.
  • the inductor magnetic core in this embodiment is manufactured using soft magnetic powder that has not been heat-treated as a raw material.
  • the present invention is not limited to this, and soft magnetism in which ⁇ Fe nanocrystals are deposited in advance by heat treatment.
  • the magnetic core of the inductor may be manufactured using powder as a raw material.
  • the inductor magnetic core can be manufactured by granulation and pressure molding in the same manner as the above-described inductor magnetic core manufacturing process.
  • the soft magnetic powder of the present embodiment is used for the dust core and the inductor core of the present embodiment manufactured as described above regardless of the manufacturing process. Similarly, the soft magnetic powder of this embodiment is used for the magnetic component of this embodiment.
  • Example 1 to 12 and Comparative Examples 1 to 8 Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 1 to 12 and Comparative Examples 1 to 8 shown in Table 1 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 1 to 12 and Comparative Examples 1 to 8 shown in Table 1, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy.
  • the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 ⁇ m. The appearance of rust generated on the surface of the produced soft magnetic powder was observed.
  • the deposited phase of the produced soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase.
  • XRD X-ray diffraction
  • the produced soft magnetic powder was heat-treated in an electric furnace at a heat treatment temperature shown in Table 1 in an argon atmosphere.
  • the saturation magnetic flux density Bs of the heat-treated soft magnetic powder was measured with a vibrating sample magnetometer (VSM). Table 1 shows the results of measurement and evaluation of the produced soft magnetic powder.
  • Comparative Example 1 As shown in Table 1, in Comparative Example 1 containing no Cr, the amorphous phase was as low as 42%, and the occurrence of rust on the surface was confirmed. Further, in Comparative Example 7 which is Fe amorphous not containing Cr, generation of rust was observed on the surface. Comparative Example 5 contained Cr, but the amorphous phase was as low as 84%. Moreover, although the comparative example 4 contained Cr, the amorphous phase was as low as 64%, and generation
  • the saturation magnetic flux density Bs was 1.32 to 1.55T. That is, all the saturation magnetic flux densities Bs of Comparative Examples 3, 5, 7, and 8 were 1.55 T or less.
  • the saturation magnetic flux density Bs was 1.56 to 1.72T. That is, all the saturation magnetic flux densities Bs of Examples 1 to 12 were 1.56 T or more.
  • Powder magnetic cores were produced from the soft magnetic powders of Examples 1 to 12 and Comparative Examples 1 to 8. Specifically, the soft magnetic powder produced by the above-described method is granulated using 2% by mass of silicone resin, and a mold having an outer diameter of 13 mm and an inner diameter of 8 mm is used with a molding pressure of 10 ton / cm 2 . Molded and cured. Then, it heat-processed with the heat processing temperature shown in Table 1 in argon atmosphere with the electric furnace, and produced the dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. Further, the obtained dust core was subjected to a constant temperature and humidity test at 60 ° C.
  • the core loss of Comparative Examples 1 to 8 was 75 to 1450 kW / m 3 .
  • the core loss of Examples 1 to 12 was 70 to 160 kW / m 3 . That is, all core losses in Examples 1 to 12 were low values. In the constant temperature and humidity test, corrosion was confirmed in Comparative Examples 1, 2, and 7, but corrosion was not confirmed in all of Examples 1 to 12.
  • the proportion of Fe in the soft magnetic powder is preferably 85 at% or less when comparing Comparative Example 1 and Comparative Example 2 from the viewpoint of generation of an amorphous phase and rust. Is done. It is understood that the ratio of Fe in the soft magnetic powder is more preferably 83.5 at% or less when Comparative Example 2 and Example 1 are compared from the viewpoint of the generation of an amorphous phase and rust. Further, it is understood that the ratio of Fe in the soft magnetic powder is preferably 78 at% or more when Example 5 and Comparative Example 3 are compared from the viewpoint of saturation magnetic flux density Bs.
  • the Fe ratio in the soft magnetic powder is more preferably 79 at% or more when Example 4 and Example 5 are compared from the viewpoint of the saturation magnetic flux density Bs. It is understood that the Fe ratio in the soft magnetic powder is more preferably 80.5 at% or more when Example 11 and Example 12 are compared from the viewpoint of the saturation magnetic flux density Bs.
  • the Si ratio in the soft magnetic powder is preferably 0.1 at% or more when Example 6 and Example 7 are compared from the viewpoint of core loss. Further, it is understood that the Si ratio in the soft magnetic powder is preferably 6 at% or less when Example 9 and Comparative Example 4 are compared from the viewpoint of core loss.
  • ⁇ T of the soft magnetic powder used for producing the dust cores of Examples 6, 7 and 8 was calculated as 89 ° C., 93 ° C. and 105 ° C., respectively. From this result, it is understood that ⁇ T increases as the proportion of Si increases. In particular, when molding a large core of about 10 g or more, it is understood that ⁇ T is preferably 100 ° C. or more, and therefore the Si ratio is more preferably 2 at% or more.
  • the ratio of B in the soft magnetic powder is preferably 10 at% or less when comparing Comparative Example 1 and Comparative Example 2 from the viewpoint of the amorphous phase and core loss.
  • the ratio of B in the soft magnetic powder is preferably 4 at% or more when Example 10 and Comparative Example 5 are compared from the viewpoint of the amorphous phase and the core loss.
  • the proportion of P in the soft magnetic powder is 12 ata when comparing Example 10, Comparative Example 5, Comparative Example 7, and Comparative Example 8 from the viewpoint of saturation magnetic flux density Bs. % Is preferred. It is understood that the ratio of P in the soft magnetic powder is more preferably 10 at% or less when Example 6, Example 10 and Comparative Example 6 are compared from the viewpoint of saturation magnetic flux density Bs. When the ratio of P in the soft magnetic powder is compared between Example 5 and Comparative Example 3 from the viewpoint of the saturation magnetic flux density Bs, it is understood that 8 at% or less is more preferable.
  • the proportion of P in the soft magnetic powder is preferably 5 at% or more when comparing Comparative Example 2 and Example 3 from the viewpoint of core loss. Further, it is more preferable that the ratio of P in the soft magnetic powder exceeds 6 at% when comparing Comparative Example 2, Example 1, Comparative Example 7 and Comparative Example 8 from the viewpoint of core loss and constant temperature and humidity test. Understood. Further, it is understood that the ratio of P in the soft magnetic powder is more preferably more than 8 at% when comparing Example 8 and Example 9 from the viewpoint of the amorphous phase and the core loss.
  • the average particle diameter of the precipitated ⁇ Fe nanocrystals was calculated to be 36 nm, and the crystallinity of the precipitated ⁇ Fe nanocrystals was calculated to be 51%.
  • the average particle diameter of the precipitated ⁇ Fe nanocrystals was calculated to be 29 nm, and the crystallinity of the precipitated ⁇ Fe nanocrystals was calculated to be 46%.
  • Examples 13 to 25 and Comparative Examples 9 and 10 Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 13 to 25 and Comparative Examples 9 and 10 shown in Table 3 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 13 to 25 and Comparative Examples 9 and 10 shown in Table 3, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy.
  • the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 ⁇ m. The appearance of rust generated on the surface of the produced soft magnetic powder was observed.
  • the deposited phase of the produced soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase.
  • XRD X-ray diffraction
  • the produced soft magnetic powder was heat-treated in an argon atmosphere at the heat treatment temperature shown in Table 3 in an argon atmosphere.
  • the saturation magnetic flux density Bs of the heat-treated soft magnetic powder was measured with a vibrating sample magnetometer (VSM). Table 3 shows the results of measurement and evaluation of the produced soft magnetic powder.
  • Powder magnetic cores were produced from the soft magnetic powders of Examples 13 to 25 and Comparative Examples 9 and 10. Specifically, the soft magnetic powder produced by the above-described method is granulated using 2% by mass of silicone resin, and a mold having an outer diameter of 13 mm and an inner diameter of 8 mm is used with a molding pressure of 10 ton / cm 2 . Molded and cured. Thereafter, heat treatment was performed in an electric furnace in an argon atmosphere at a heat treatment temperature shown in Table 3 to produce a dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. The obtained powder magnetic core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. Table 4 shows the results of measurement and evaluation of the produced dust core.
  • the comparison between Comparative Example 9 and Example 13 shows that even when Cr is added slightly, the proportion of the amorphous phase in the soft magnetic powder is remarkably improved, and the effect of rust prevention.
  • the Cr content in the soft magnetic powder is preferably 3 at% or less.
  • the Cr ratio in the soft magnetic powder is more preferably 1.8 at% or less, and further preferably 1.5 at% or less.
  • the Cr content in the soft magnetic powder is preferably 0.1 at% or more. It is understood that the ratio of Cr in the soft magnetic powder is more preferably 0.5 at% or more when Example 14 and Example 15 are compared from the viewpoint of core loss.
  • the proportion of Cu in the soft magnetic powder is preferably less than 0.7 at% when comparing Example 15 and Example 23 from the viewpoint of the amorphous phase and the core loss. It is understood that the ratio of Cu in the soft magnetic powder is more preferably 0.65 at% or less when Example 15 and Example 16 are compared from the viewpoint of the amorphous phase and the core loss. Further, it is understood from the comparison between Comparative Example 10 and Example 25 that the Cu ratio in the soft magnetic powder is preferably 0.4 at% or more. From the comparison between Example 24 and Example 25, it is understood that the ratio of Cu in the soft magnetic powder is more preferably 0.5 at% or more.
  • Examples 26 to 36 As raw materials for the soft magnetic powders of Examples 26 to 36 shown in Table 5 below, industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, ferrochrome, ferrocarbon, niobium, molybdenum, Co, Ni, tin, zinc , Mn was prepared. The raw materials were weighed so as to have the alloy compositions of Examples 26 to 36 shown in Table 5, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 ⁇ m. The appearance of rust generated on the surface of the produced soft magnetic powder was observed.
  • the deposited phase of the produced soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase.
  • XRD X-ray diffraction
  • the produced soft magnetic powder was heat-treated in an argon atmosphere in an argon atmosphere at a heat treatment temperature shown in Table 5.
  • the saturation magnetic flux density Bs of the heat-treated soft magnetic powder was measured with a vibrating sample magnetometer (VSM). Table 5 shows the results of measurement and evaluation of the produced soft magnetic powder.
  • Examples 26 to 36 addition of M element (C Cincinnati, Ni, Cu, Zn, Mn) and substitution of Fe with Nb, Mo, Sn, C, etc. are performed. As shown in Table 5, in Examples 26 to 36, no rust was observed on the surface, and the saturation magnetic flux density Bs was 1.58 to 1.72 T. From the comparison of Examples 26, 29 and 31, it can be understood that when C is replaced with Fe, the amorphous ratio can be kept high even when the ratio of Fe is high. Further, from Example 32, it is understood that the saturation magnetic flux density Bs is improved when Co is added.
  • a dust core was prepared from the soft magnetic powders of Examples 26 to 36. Specifically, the soft magnetic powder produced by the method described above, and granulated using a 2 wt% silicone resin, the molding pressure of 10ton / cm 2 using a mold having an outer diameter of 13mm and inner diameter of 8mm Molded and cured. Then, it heat-processed with the heat processing temperature shown in Table 5 in argon atmosphere with the electric furnace, and produced the dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. The obtained powder magnetic core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. Table 6 shows the results of measurement and evaluation of the produced dust core.
  • Example 37 to 45 Industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, and ferrochrome were prepared as raw materials for the soft magnetic powders of Examples 37 to 45 and Comparative Example 11 shown in Table 7 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 37 to 45 and Comparative Example 11 shown in Table 7, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy.
  • the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 ⁇ m.
  • the produced soft magnetic powder was granulated using 2% by mass of a silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment. . Thereafter, heat treatment was performed in an electric furnace in an argon atmosphere at a heat treatment temperature shown in Table 7 to produce a dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer.
  • the average particle diameter and crystallinity of the ⁇ Fe nanocrystals in the soft magnetic powder contained in the dust core were calculated.
  • Table 7 shows the results of measurement and evaluation of the produced dust core.
  • the average particle diameter of the ⁇ Fe nanocrystals, the crystallinity of the ⁇ Fe nanocrystals, and the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystals are expressed as ⁇ Fe crystal particle diameter, ⁇ Fe, respectively. It is expressed as crystallinity and compound phase crystallinity.
  • Examples 37 to 42 have the same elemental composition, but only the heat treatment conditions are different.
  • Examples 43 to 45 also have the same elemental composition, but only the heat treatment conditions are different.
  • Table 7 shows that even in a dust core made of soft magnetic powder having the same elemental composition, due to the difference in heat treatment conditions, the core loss, the crystal grain size and crystallinity of ⁇ Fe nanocrystals, In addition, it is understood that the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystal is greatly different.
  • the core loss increases when the crystal grain size of ⁇ Fe nanocrystals becomes coarse as in Comparative Example 11. I understand. Therefore, it is understood that the crystal grain size of the ⁇ Fe nanocrystal is preferably 50 nm or less.
  • Example 37 and Example 43 are compared from the viewpoint of the crystallinity of the core loss and the ⁇ Fe nanocrystal, when the crystallinity of the ⁇ Fe nanocrystal is low as in Example 43, the magnetostriction is sufficiently reduced. It can be seen that the core loss increases. Therefore, it is understood that the crystallinity of ⁇ Fe nanocrystals is preferably 35% or more.
  • the crystallinity of the compound phase other than the bcc phase in the ⁇ Fe nanocrystal is preferably 7% or less, more preferably 5% or less, and still more preferably 3% or less. It is understood.
  • Example 46 to 66 Industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, ferrochrome, and Mn, Al, Ti, FeS were prepared as raw materials for the soft magnetic powders of Examples 46 to 66 shown in Table 8 below.
  • the raw materials were weighed so as to have the alloy compositions of Examples 46 to 66 shown in Table 8, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 ⁇ m.
  • the appearance of rust produced on the surfaces of the soft magnetic powders of Examples 46 to 66 was observed.
  • the precipitated phase of the soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase.
  • XRD X-ray diffraction
  • the produced soft magnetic powder was heat-treated in an electric furnace in an argon atmosphere at the heat treatment temperature shown in Table 9, and the heat-treated soft magnetic powder was subjected to a saturation magnetic flux density Bs with a vibrating sample magnetometer (VSM). Was measured.
  • Table 9 shows the results of measurement and evaluation of the produced soft magnetic powder.
  • dust cores were produced from the soft magnetic powders of Examples 46 to 66.
  • the soft magnetic powder produced by the above-described method is granulated using 2% by mass of silicone resin, and a mold having an outer diameter of 13 mm and an inner diameter of 8 mm is used with a molding pressure of 10 ton / cm 2 . Molded and cured. Thereafter, heat treatment was performed at a heat treatment temperature shown in Table 9 in an argon atmosphere in an electric furnace to produce a dust core.
  • the core loss of 20 kHz-100 mT was measured using the AC BH analyzer.
  • the obtained powder magnetic core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. Table 9 shows the results of measurement and evaluation of the produced dust core.
  • Examples 46 to 66 contain Al, Ti, S, N, and O as trace elements in various contents.
  • Examples 46 to 62 have the same elemental composition of Fe, Si, B, P, Cu and Cr. From Table 9, it is understood that the ratio of the amorphous phase shows a high value of 92% or more for Examples 46, 48, 49, and 51 to 66. Also, from Table 9, it is understood that the saturation magnetic flux density Bs shows a good value of 1.58 T or more for Examples 46 to 52 and 54 to 66. Furthermore, it can be seen from Table 9 that the core loss shows a good value of 220 kW / m 3 or less for Examples 46, 48, 49, 51 to 58, and 60 to 66.
  • the saturation magnetic flux density Bs of Examples 47, 50, 53, and 59 having a large content of Al, Ti, S, and O is low in the trace element content. Compared to the rest of the examples. However, it is understood that the saturation magnetic flux density Bs of Example 47, Example 50, Example 53, and Example 59 shows a value of 1.54 T or more.
  • Example 46 and Examples 47 to 49 it can be understood that as the Al content increases, the amorphous ratio and the saturation magnetic flux density Bs decrease, and the core loss increases. That is, the content of Al is preferably 0.05% by mass or less from the viewpoint of amorphous ratio, saturation magnetic flux density Bs and core loss, and 0.005% by mass or less from the viewpoint of core loss reduction. It is understood that there is more preferred.
  • the content of Ti is preferably 0.05% by mass or less from the viewpoint of amorphous ratio, saturation magnetic flux density Bs and core loss, and 0.005% by mass or less from the viewpoint of core loss reduction. It is understood that there is more preferred.
  • the amorphous ratio and the saturation magnetic flux density Bs decrease as the S content increases.
  • the content of S is preferably 0.5% by mass or less from the viewpoint of the amorphous ratio and the saturation magnetic flux density Bs, and more preferably 0.05% by mass or less from the viewpoint of corrosion resistance. It is understood that it is preferable.
  • Example 46 it is understood that as the N content increases, the amorphous ratio decreases and the core loss increases. That is, it is understood that the N content is preferably 0.01% by mass or less and more preferably 0.002% by mass or less from the viewpoint of the amorphous ratio and the core loss.
  • Example 59 it is understood that the corrosion resistance decreases as the O content increases. That is, it is understood that the content of O is preferably 1% by mass or less and more preferably 0.3% by mass or less from the viewpoint of corrosion resistance.
  • inductor An inductor was fabricated using the soft magnetic powder of the present embodiment, and the DC superposition characteristics of the fabricated inductor were evaluated. The method for manufacturing the inductor will be described in detail below.
  • a mixture of B and a binder was granulated to produce a granulated powder.
  • the silicone resin as a binder was added so as to be 2% by mass with respect to the total amount of the soft magnetic powder A and the soft magnetic powder B.
  • the coil 120 shown in FIG. 1 was prepared as a coil.
  • This coil 120 is obtained by winding a flat conducting wire 121 edgewise, and the number of turns is 3.5 turns.
  • the flat conducting wire 121 is a rectangle having a cross-sectional shape of 2.0 mm ⁇ 0.6 mm, and has an insulating layer made of polyamideimide having a thickness of 20 ⁇ m on the surface.
  • the coil 120 has surface mounting terminals 122 at both ends. With the coil 120 placed in the mold in advance, the above-mentioned granulated powder is filled in the mold cavity, and the granulated powder and the coil 120 are integrally pressure-molded by a molding pressure of 5 ton / cm 2.
  • the molded body was heat-treated in an electric furnace in an argon atmosphere at 400 ° C. for 30 minutes, and the inductor 100 of the example in which the coil 120 was embedded inside the dust core 110 was produced.
  • the inductor 100A of the comparative example Fe—Si—Cr powder is used instead of the soft magnetic powders A and B, and the same manufacturing method as that of the inductor 100 of the above-described embodiment is used.
  • An inductor 100A in which the coil 120 was embedded was manufactured. Since the coil 120 of the inductor 100A of the comparative example has the same structure as the coil 120 of the inductor 100 of the embodiment, detailed description thereof is omitted.
  • the inductor 100 is an integrally molded inductor 100 in which a coil 120 is embedded in a dust core 110. Further, the surface mounting terminal 122 of the coil 120 is drawn to the outside of the dust core 110.
  • the inductor 100A of the comparative example is an integrally molded inductor 100A in which the coil 120 is embedded in the dust core 110A, like the inductor 100 of the embodiment.
  • the surface mounting terminal 122 of the coil 120 is drawn out of the dust core 110A.
  • FIG. 4 shows the DC superposition characteristics of the inductors 100 and 100A of the example and the comparative example. From FIG. 4, it is understood that the inductor 100 of the example has a smaller rate of decrease of the inductance L due to the increase of the applied current I than the inductor 100A of the comparative example. That is, it can be understood that the inductor 100 of the example exhibits superior DC superposition characteristics as compared with the inductor 100A of the comparative example.
  • the present invention relates to Japanese Patent Application No. 2017-27162 filed with the Japan Patent Office on February 16, 2017 and Japanese Patent Application No. 2017-206608 filed with the Japan Patent Office on October 25, 2017. The contents of which are incorporated herein by reference.

Abstract

A soft magnetic powder is represented by the chemical composition formula FeaSibBcPdCreMf with the remainder made up by unavoidable impurities. In the chemical composition formula, M represents at least one element selected from V, Mn, Co, Ni, Cu and Zn; 0 at% ≤ b ≤ 6 at%; 4 at% ≤ c ≤ 10 at%; 5 at% ≤ d ≤ 12 at%; 0 at% < e; 0.4 at% ≤ f < 6 at%; and a + b + c + d + e + f = 100 at%.

Description

軟磁性粉末、圧粉磁芯、磁性部品及び圧粉磁芯の製造方法Soft magnetic powder, dust core, magnetic component, and method for manufacturing dust core
　本発明は、圧粉磁芯等の磁性部品への使用に適している軟磁性粉末に関する。 The present invention relates to a soft magnetic powder suitable for use in magnetic parts such as a dust core.
　特許文献１には、Ｆｅ、Ｓｉ、Ｂ及びＣｕからなる軟磁性合金が開示されている。特許文献１の軟磁性合金は、所定の元素組成を有する合金溶湯をロール急冷法により急冷して薄帯として作製されている。また、特許文献２には、実施例５としてＦｅbalＳｉ１０Ｂ１１Ｐ５Ｃｒ０．５にＣｕを０．０９質量％含む元素組成の軟磁性粉末が開示されている。特許文献２の軟磁性粉末の製造工程では、水アトマイズ法が急冷方法として採用されている。 Patent Document 1 discloses a soft magnetic alloy made of Fe, Si, B, and Cu. The soft magnetic alloy of Patent Document 1 is manufactured as a ribbon by quenching a molten alloy having a predetermined element composition by a roll quenching method. Patent Document 2 discloses as Example 5 a soft magnetic powder having an elemental composition containing 0.09% by mass of Cu in Fe bal Si 10 B 11 P 5 Cr 0.5 . In the manufacturing process of the soft magnetic powder of Patent Document 2, the water atomization method is adopted as the rapid cooling method.
特開２０１１－１４９０４５号公報JP 2011-149045 A 特開２００９－１７４０３４号公報JP 2009-174034 A
　圧粉磁芯等の磁性部品に使用される軟磁性合金の形態としては、所望の形状への成形の容易性から粉末が求められている。ここで特許文献１の軟磁性合金の薄帯から軟磁性粉末を作製する場合には、粉砕工程が別途必要となり、プロセスが煩雑になると同時に球状粉末の作製が難しく成形性に劣るという問題がある。また、特許文献１の軟磁性合金の製造工程において水アトマイズ法やガスアトマイズ後に水で急冷する方法を採用した場合、軟磁性粉末を合金溶湯から直接的に得ることができるため、簡略化された工程で軟磁性粉末を作製できる利点がある。しかしながら、特許文献１の軟磁性合金は防錆性を持たせる元素であるＣｒを含有していないため、水で処理した際に粉体に錆が発生する可能性があり、作製された軟磁性粉末の信頼性に欠ける。一方、特許文献２の実施例５の軟磁性粉末は、防錆性を持たせる元素であるＣｒを含有しているが、ＳｉやＢを多量に含有していることから軟磁気特性が劣化する可能性がある。 As a form of a soft magnetic alloy used for a magnetic part such as a dust core, powder is required from the viewpoint of ease of forming into a desired shape. Here, when the soft magnetic powder is produced from the thin ribbon of the soft magnetic alloy of Patent Document 1, a pulverization step is separately required, and the process becomes complicated, and at the same time, the production of the spherical powder is difficult and the formability is poor. . In addition, when employing a water atomization method or a method of quenching with water after gas atomization in the manufacturing process of the soft magnetic alloy of Patent Document 1, since the soft magnetic powder can be obtained directly from the molten alloy, a simplified process There is an advantage that soft magnetic powder can be produced. However, since the soft magnetic alloy of Patent Document 1 does not contain Cr, which is an element imparting rust prevention, rust may be generated in the powder when treated with water, and the produced soft magnetic alloy Lack of powder reliability. On the other hand, the soft magnetic powder of Example 5 of Patent Document 2 contains Cr, which is an element that imparts rust prevention properties, but soft magnetic properties deteriorate because it contains a large amount of Si and B. there is a possibility.
　そこで、本発明は、防錆性と軟磁気特性とを高度に両立した軟磁性粉末を提供することを目的とする。 Therefore, an object of the present invention is to provide a soft magnetic powder that is highly compatible with rust prevention and soft magnetic properties.
　　本発明の一の側面は、第１の軟磁性粉末として、
　不可避不純物を除き組成式ＦｅａＳｉｂＢｃＰｄＣｒｅＭｆで表される軟磁性粉末であって、
　Ｍは、Ｖ、Ｍｎ、Ｃｏ、Ｎｉ、Ｃｕ、Ｚｎから選ばれる１種以上の元素であり、
　０ａｔ％≦ｂ≦６ａｔ％、４ａｔ％≦ｃ≦１０ａｔ％、５ａｔ％≦ｄ≦１２ａｔ％、０ａｔ％＜ｅ、０．４ａｔ％≦ｆ＜６ａｔ％、且つ、ａ＋ｂ＋ｃ＋ｄ＋ｅ＋ｆ＝１００ａｔ％である軟磁性粉末を提供する。 One aspect of the present invention is the first soft magnetic powder,
A soft magnetic powder represented by the composition formula Fe a Si b B c P d Cr e M f excluding inevitable impurities,
M is one or more elements selected from V, Mn, Co, Ni, Cu, Zn,
Soft magnetic powder with 0 at% ≦ b ≦ 6 at%, 4 at% ≦ c ≦ 10 at%, 5 at% ≦ d ≦ 12 at%, 0 at% <e, 0.4 at% ≦ f <6 at%, and a + b + c + d + e + f = 100 at% I will provide a.
　本発明による軟磁性粉末は、所定範囲のＦｅ、Ｓｉ、Ｂ、Ｐ、Ｃｒ及びＭ（Ｖ、Ｍｎ、Ｃｏ、Ｎｉ、Ｃｕ、Ｚｎから選ばれる１種以上の元素）を含んでいるため、Ｃｒを含む酸化被膜が粉体の表面に形成されており、且つ、非晶質相を高い割合で含有することができる。これにより、本発明の軟磁性粉末においては、防錆性と軟磁気特性とが高度に両立されている。また、本発明の軟磁性粉末は防錆性を有していることから、本発明の軟磁性粉末の製造工程においては、量産性に優れ冷却性能の高い水などの冷媒を用いた急冷方法を採用することができる。 The soft magnetic powder according to the present invention contains a predetermined range of Fe, Si, B, P, Cr, and M (one or more elements selected from V, Mn, Co, Ni, Cu, and Zn). Is formed on the surface of the powder, and an amorphous phase can be contained in a high proportion. Thereby, in the soft magnetic powder of this invention, rust prevention property and soft magnetic characteristic are highly compatible. In addition, since the soft magnetic powder of the present invention has rust prevention properties, in the manufacturing process of the soft magnetic powder of the present invention, a rapid cooling method using a coolant such as water having excellent mass productivity and high cooling performance is used. Can be adopted.
　添付の図面を参照しながら下記の最良の実施の形態の説明を検討することにより、本発明の目的が正しく理解され、且つその構成についてより完全に理解されるであろう。 DETAILED DESCRIPTION OF THE INVENTION By studying the following description of the best mode with reference to the accompanying drawings, the object of the present invention will be understood correctly and the configuration thereof will be more fully understood.
本発明の実施の形態によるインダクタを示す斜視図である。図において、圧粉磁芯の輪郭は点線で描画されている。It is a perspective view which shows the inductor by embodiment of this invention. In the figure, the outline of the dust core is drawn with a dotted line. 図１のインダクタを示す側面図である。図において、圧粉磁芯の輪郭は点線で描画されている。It is a side view which shows the inductor of FIG. In the figure, the outline of the dust core is drawn with a dotted line. 比較例のインダクタを示す斜視図である。図において、圧粉磁芯の輪郭は点線で描画されている。It is a perspective view which shows the inductor of a comparative example. In the figure, the outline of the dust core is drawn with a dotted line. 図１及び図３のインダクタの直流重畳特性を示すグラフである。グラフ中において、実施例を実線で、比較例を破線で、夫々示している。It is a graph which shows the direct current | flow superimposition characteristic of the inductor of FIG.1 and FIG.3. In the graph, an example is indicated by a solid line, and a comparative example is indicated by a broken line.
　本発明については多様な変形や様々な形態にて実現することが可能であるが、その一例として、図面に示すような特定の実施の形態について、以下に詳細に説明する。図面及び実施の形態は、本発明をここに開示した特定の形態に限定するものではなく、添付の請求の範囲に明示されている範囲内においてなされる全ての変形例、均等物、代替例をその対象に含むものとする。 The present invention can be realized in various modifications and various forms. As an example, specific embodiments as shown in the drawings will be described in detail below. The drawings and the embodiments are not intended to limit the invention to the specific forms disclosed herein, but to all modifications, equivalents, alternatives made within the scope of the appended claims. It shall be included in the object.
　本実施の形態による軟磁性粉末は、不可避不純物を除き組成式ＦｅａＳｉｂＢｃＰｄＣｒｅＭｆで表される。組成式ＦｅａＳｉｂＢｃＰｄＣｒｅＭｆにおいて、Ｍは、Ｖ、Ｍｎ、Ｃｏ、Ｎｉ、Ｃｕ、Ｚｎから選ばれる１種以上の元素であり、０ａｔ％≦ｂ≦６ａｔ％、４ａｔ％≦ｃ≦１０ａｔ％、５ａｔ％≦ｄ≦１２ａｔ％、０ａｔ％＜ｅ、０．４ａｔ％≦ｆ＜６ａｔ％、且つ、ａ＋ｂ＋ｃ＋ｄ＋ｅ＋ｆ＝１００ａｔ％である。 Soft magnetic powder according to the present embodiment is expressed by a composition formula except inevitable impurities Fe a Si b B c P d Cr e M f. In the composition formula Fe a Si b B c P d Cr e M f , M is one or more elements selected from V, Mn, Co, Ni, Cu, and Zn, and 0 at% ≦ b ≦ 6 at%, 4 at. % ≦ c ≦ 10 at%, 5 at% ≦ d ≦ 12 at%, 0 at% <e, 0.4 at% ≦ f <6 at%, and a + b + c + d + e + f = 100 at%.
　本実施の形態の軟磁性粉末は、様々な磁性部品や圧粉磁芯、インダクタの磁芯を作製するための直接的な材料として使用可能である。 The soft magnetic powder of this embodiment can be used as a direct material for producing various magnetic parts, dust cores, and inductor cores.
　本実施の形態の軟磁性粉末は、アトマイズ法等の製造方法によって作製することができる。このようにして作製された軟磁性粉末は、非晶質相（アモルファス相）を主相としている。また本発明の軟磁性粉末は、ナノ結晶を含有していることが好ましい。ここで、ナノ結晶を含有する軟磁性粉末は、後述のように軟磁性粉末に所定の熱処理条件による熱処理を施してｂｃｃＦｅ（αＦｅ）のナノ結晶を析出させることにより得られる。 The soft magnetic powder of the present embodiment can be manufactured by a manufacturing method such as an atomizing method. The soft magnetic powder thus produced has an amorphous phase as the main phase. The soft magnetic powder of the present invention preferably contains nanocrystals. Here, the soft magnetic powder containing nanocrystals is obtained by subjecting the soft magnetic powder to heat treatment under predetermined heat treatment conditions to precipitate bccFe (αFe) nanocrystals as described later.
　一般的に、軟磁性粉末をＡｒガス雰囲気のような不活性雰囲気中で熱処理した場合、結晶化が２回以上確認できる。最初に結晶化が開始する温度を第１結晶化開始温度（Ｔｘ１）といい、２回目の結晶化が開始する温度を第２結晶化開始温度（Ｔｘ２）という。また、第１結晶化開始温度（Ｔｘ１）と第２結晶化開始温度（Ｔｘ２）の間の温度差をΔＴ＝Ｔｘ２－Ｔｘ１という。第１結晶化開始温度（Ｔｘ１）は、αＦｅのナノ結晶析出の発熱ピークであり、第２結晶化開始温度（Ｔｘ２）は、ＦｅＢやＦｅＰ等の化合物析出の発熱ピークである。これらの結晶化開始温度は、例えば、示差走査熱量分析（ＤＳＣ）装置を使用して、４０℃／分程度の昇温速度で熱分析を行うことで評価可能である。 Generally, when a soft magnetic powder is heat-treated in an inert atmosphere such as an Ar gas atmosphere, crystallization can be confirmed twice or more. The temperature at which crystallization starts first is called the first crystallization start temperature (Tx1), and the temperature at which the second crystallization starts is called the second crystallization start temperature (Tx2). The temperature difference between the first crystallization start temperature (Tx1) and the second crystallization start temperature (Tx2) is referred to as ΔT = Tx2−Tx1. The first crystallization start temperature (Tx1) is an exothermic peak of αFe nanocrystal precipitation, and the second crystallization start temperature (Tx2) is an exothermic peak of precipitation of compounds such as FeB and FeP. These crystallization start temperatures can be evaluated, for example, by performing thermal analysis at a rate of temperature increase of about 40 ° C./min using a differential scanning calorimetry (DSC) apparatus.
　軟磁性粉末においてαＦｅのナノ結晶を析出させるためには、化合物相の析出を抑制するように、第２結晶化開始温度（Ｔｘ２）以下の温度で熱処理することが望ましい。ここでΔＴが大きい場合、所定の熱処理条件における熱処理が容易になる。このため、熱処理によってαＦｅのナノ結晶のみを析出させて良好な軟磁気特性の軟磁性粉末を得ることができる。即ち、ΔＴが大きくなるように軟磁性粉末の元素組成を調整して熱処理することにより、軟磁性粉末に含まれるαＦｅのナノ結晶組織が安定し、αＦｅのナノ結晶を含む軟磁性粉末を備える圧粉磁芯やインダクタの磁芯のコアロスも低減することとなる。 In order to precipitate αFe nanocrystals in the soft magnetic powder, it is desirable to perform heat treatment at a temperature equal to or lower than the second crystallization start temperature (Tx2) so as to suppress the precipitation of the compound phase. Here, when ΔT is large, heat treatment under a predetermined heat treatment condition is facilitated. Therefore, only αFe nanocrystals can be precipitated by heat treatment to obtain a soft magnetic powder having good soft magnetic properties. That is, by adjusting the elemental composition of the soft magnetic powder so that ΔT is increased and heat-treating, the αFe nanocrystal structure contained in the soft magnetic powder is stabilized, and the pressure provided with the soft magnetic powder containing the αFe nanocrystal is stabilized. The core loss of the magnetic core of the powder magnetic core or the inductor is also reduced.
　以下、本実施の形態による軟磁性粉末の組成範囲について更に詳しく説明する。 Hereinafter, the composition range of the soft magnetic powder according to the present embodiment will be described in more detail.
　本実施の形態による軟磁性粉末において、Ｆｅ元素は主元素であり、磁性を担う必須元素である。軟磁性粉末の飽和磁束密度Ｂｓの向上及び原料価格の低減のためには、基本的にはＦｅの割合が多い方が好ましい。Ｆｅの割合は、軟磁性粉末において高い飽和磁束密度Ｂｓを得るため、７８ａｔ％以上とすることが好ましく、また８５ａｔ％以下とすることが好ましい。Ｆｅの割合が７８ａｔ％以上の場合、上述の効果に加えて、ΔＴを大きくできる。Ｆｅの割合の増加により飽和磁束密度Ｂｓを更に向上させるため、７９ａｔ％以上であることがより好ましく、８０．５ａｔ％以上が更に好ましい。しかしながら、Ｆｅの割合が８５ａｔ％を超えると、Ｆｅ量が過多となって非晶質相が９０％以上の軟磁性粉末が得られない。また非晶質相の割合が高い軟磁性粉末を安定的に得るためには、Ｆｅの割合を８３．５ａｔ％以下とすることが好ましい。 In the soft magnetic powder according to the present embodiment, the Fe element is a main element and an essential element responsible for magnetism. In order to improve the saturation magnetic flux density Bs of the soft magnetic powder and reduce the raw material price, it is basically preferable that the ratio of Fe is large. In order to obtain a high saturation magnetic flux density Bs in the soft magnetic powder, the proportion of Fe is preferably 78 at% or more, and preferably 85 at% or less. In the case where the ratio of Fe is 78 at% or more, ΔT can be increased in addition to the above effects. In order to further improve the saturation magnetic flux density Bs by increasing the proportion of Fe, it is more preferably 79 at% or more, and further preferably 80.5 at% or more. However, if the proportion of Fe exceeds 85 at%, the amount of Fe becomes excessive and a soft magnetic powder having an amorphous phase of 90% or more cannot be obtained. In order to stably obtain a soft magnetic powder having a high amorphous phase ratio, the Fe ratio is preferably 83.5 at% or less.
　本実施の形態による軟磁性粉末において、Ｓｉ元素は非晶質相形成を担う元素であり、ナノ結晶化にあたってはナノ結晶の安定化に寄与する。Ｓｉの割合は、圧粉磁芯やインダクタの磁芯のコアロスを低減するため、６ａｔ％以下（ゼロを含む）とする必要がある。Ｓｉの割合が６ａｔ％を超えるとＳｉ量が過多のためアモルファス形成能が低下し非晶質相が９０％以上の軟磁性粉末が得られない。一方、少量のＳｉ量においてもアモルファス形成能の向上に効果があることや、原料の溶解時の安定性を考慮すると、Ｓｉを含有することが好ましく、Ｓｉの割合は０．１ａｔ％以上であることがより好ましい。加えて、Ｓｉの割合は、ΔＴを大きくするため、２ａｔ％以上であることがより好ましい。 In the soft magnetic powder according to the present embodiment, the Si element is an element responsible for forming an amorphous phase, and contributes to the stabilization of the nanocrystal in the nanocrystallization. The Si ratio needs to be 6 at% or less (including zero) in order to reduce the core loss of the dust core and the inductor core. When the proportion of Si exceeds 6 at%, the amount of Si is excessive, so that the amorphous forming ability is lowered, and a soft magnetic powder having an amorphous phase of 90% or more cannot be obtained. On the other hand, considering the effect of improving the amorphous forming ability even with a small amount of Si and the stability during melting of the raw material, it is preferable to contain Si, and the proportion of Si is 0.1 at% or more It is more preferable. In addition, the ratio of Si is more preferably 2 at% or more in order to increase ΔT.
　本実施の形態による軟磁性粉末において、Ｂ元素は非晶質相形成を担う必須元素である。Ｂの割合は、軟磁性粉末の非晶質相を９０％以上として圧粉磁芯やインダクタの磁芯のコアロスを低減するため、４ａｔ％以上かつ１０ａｔ％以下とする必要がある。Ｂの割合が１０ａｔ％を超えると、合金溶湯の融点が急激に高くなり製造上好ましくなく、アモルファス形成能も低下する。一方、Ｂの割合が４ａｔ％より小さくなると、メタロイド元素であるＳｉ、Ｂ、Ｐのバランスが悪くなりアモルファス形成能が低下する。 In the soft magnetic powder according to the present embodiment, the B element is an essential element responsible for forming an amorphous phase. The ratio of B needs to be 4 at% or more and 10 at% or less in order to reduce the core loss of the powder magnetic core or the magnetic core of the inductor by setting the amorphous phase of the soft magnetic powder to 90% or more. If the ratio of B exceeds 10 at%, the melting point of the molten alloy increases rapidly, which is not preferable for production, and the amorphous forming ability is also lowered. On the other hand, when the ratio of B becomes smaller than 4 at%, the balance of Si, B, and P, which are metalloid elements, is deteriorated and the amorphous forming ability is lowered.
　本実施の形態による軟磁性粉末において、Ｐ元素は非晶質相形成を担う必須元素である。前述のように、本実施の形態によるＰの割合は、５ａｔ％以上且つ１２ａｔ％以下である。Ｐの割合が５ａｔ％以上となると、アモルファス形成能が向上して非晶質相が多くなり、安定した軟磁気特性が得られる。一方、Ｐの割合が１２ａｔ％を超えると、メタロイド元素であるＳｉ、Ｂ、Ｐのバランスが悪くなりアモルファス形成能が低下すると同時に飽和磁束密度Ｂｓが著しく低下する。またＰの割合を１０ａｔ％以下にすると、飽和磁束密度Ｂｓの低下が抑制できるため好ましい。更に、Ｐの割合を８ａｔ％以下にすると、熱処理後に均一なナノ組織が得られやすく、良好な軟磁気特性を得られるため、より好ましい。一方、Ｐの割合が５ａｔ％を超えると、アモルファス形成能が向上してより安定な軟磁気特性が得られるため好ましい。また、Ｐの割合が、６ａｔ％を超えると耐食性が著しく向上し、８ａｔ％を超えるとアトマイズ時の軟磁性粉末の球状化が進むため充填率が向上し、また耐食性が更に高まって、熱処理後に均一なナノ組織が得られやすいため、より好ましい。 In the soft magnetic powder according to the present embodiment, the P element is an essential element for forming an amorphous phase. As described above, the proportion of P according to the present embodiment is not less than 5 at% and not more than 12 at%. When the proportion of P is 5 at% or more, the amorphous forming ability is improved, the amorphous phase is increased, and stable soft magnetic characteristics can be obtained. On the other hand, when the proportion of P exceeds 12 at%, the balance of the metalloid elements Si, B, and P is deteriorated, the amorphous forming ability is lowered, and at the same time, the saturation magnetic flux density Bs is significantly lowered. Moreover, it is preferable to set the ratio of P to 10 at% or less because a decrease in saturation magnetic flux density Bs can be suppressed. Furthermore, it is more preferable that the ratio of P is 8 at% or less because a uniform nanostructure can be easily obtained after heat treatment and good soft magnetic properties can be obtained. On the other hand, when the ratio of P exceeds 5 at%, it is preferable because amorphous forming ability is improved and more stable soft magnetic characteristics can be obtained. In addition, when the ratio of P exceeds 6 at%, the corrosion resistance is remarkably improved, and when it exceeds 8 at%, the soft magnetic powder at the time of atomization progresses to spheroidize, so that the filling rate is improved and the corrosion resistance is further increased. It is more preferable because a uniform nanostructure can be easily obtained.
　本実施の形態による軟磁性粉末において、Ｃｒ元素は防錆性に寄与する必須元素である。前述のように、本実施の形態によるＣｒの割合は、０ａｔ％よりも大きい。詳しくは、Ｃｒの割合が０ａｔ％よりも大きい場合、軟磁性粉末の粉体の表面に酸化被膜が形成されるため防錆性が付与され、また非晶質相の割合が向上する。軟磁性粉末の粉体の表面に酸化被膜が形成されるため、軟磁性粉末を水を用いた冷却法で作製する場合においても、作製された軟磁性粉末の粉体の表面に錆が生じることはない。一方、Ｃｒの割合は、軟磁性粉末において高い飽和磁束密度Ｂｓを得るため３ａｔ％以下とすることが好ましく、コアロスの低減を考慮すると１．８ａｔ％以下とするのがより好ましい。また、Ｃｒの割合は、高い飽和磁束密度Ｂｓを得るためには１．５ａｔ％以下とすることが好ましく、より高い飽和磁束密度Ｂｓを得るためには１．０ａｔ％以下とすることがより好ましい。加えて、Ｃｒの割合は、防錆性を向上させるため、０．１ａｔ％以上であることが好ましく、０．５ａｔ％以上がより好ましい。 In the soft magnetic powder according to the present embodiment, Cr element is an essential element contributing to rust prevention. As described above, the proportion of Cr according to the present embodiment is greater than 0 at%. Specifically, when the proportion of Cr is greater than 0 at%, an oxide film is formed on the surface of the soft magnetic powder, so that rust prevention is imparted and the proportion of the amorphous phase is improved. Since an oxide film is formed on the surface of the soft magnetic powder, rust occurs on the surface of the soft magnetic powder even when the soft magnetic powder is manufactured by a cooling method using water. There is no. On the other hand, the Cr ratio is preferably 3 at% or less in order to obtain a high saturation magnetic flux density Bs in the soft magnetic powder, and more preferably 1.8 at% or less in consideration of reduction of core loss. The Cr ratio is preferably 1.5 at% or less in order to obtain a high saturation magnetic flux density Bs, and more preferably 1.0 at% or less in order to obtain a higher saturation magnetic flux density Bs. . In addition, the ratio of Cr is preferably 0.1 at% or more, and more preferably 0.5 at% or more in order to improve rust prevention.
　本実施の形態による軟磁性粉末において、Ｍ元素は必須元素である。本実施の形態によるＭの割合は、０．４ａｔ％以上かつ６ａｔ％未満である。Ｍ元素とＰ元素との同時添加により、耐食性が著しく向上する。詳しくは、Ｍの割合は、軟磁性粉末におけるナノ結晶の粗大化を防止して圧粉磁芯において所望のコアロスを得るため、０．４ａｔ％以上とする必要があり、十分なアモルファス形成能によって非晶質相を９０％以上とするため、６ａｔ％未満とする必要がある。 M element is an essential element in the soft magnetic powder according to the present embodiment. The proportion of M according to the present embodiment is 0.4 at% or more and less than 6 at%. By simultaneous addition of M element and P element, the corrosion resistance is remarkably improved. Specifically, the proportion of M needs to be 0.4 at% or more in order to prevent the coarsening of the nanocrystals in the soft magnetic powder and obtain a desired core loss in the dust core. In order to make the amorphous phase 90% or more, it is necessary to make it less than 6 at%.
　本実施の形態のＭ元素には、Ｃｕを０．４ａｔ％以上且つ０．７ａｔ％未満で含むことが好ましい。より詳しくは、ＭｆはＣｕｇＭ´ｈで表され、Ｍ´はＶ、Ｍｎ、Ｃｏ、Ｎｉ、Ｚｎから選ばれる１種以上の元素であり、０．４ａｔ％≦ｇ＜０．７ａｔ％、且つｆ＝ｇ＋ｈを満たしていることが好ましい。Ｍ元素が上記の条件を満たすことにより、軟磁性粉末において防錆性の向上及びアモルファス形成能の増大が更に図られることとなる。Ｃｕの割合を０．７ａｔ％未満とすると、非晶質相の割合の高い粉末が得られるため好ましく、０．６５ａｔ％以下がより好ましい。また、Ｃｕの割合を０．４ａｔ％以上とすると、αＦｅのナノ結晶の析出量が多くなり均一なナノ組織を得やすいので好ましく、０．５ａｔ％以上とすると、耐食性が著しく向上すると共にαＦｅのナノ結晶の析出量が更に増加して軟磁気特性が向上するため、より好ましい。 The M element in the present embodiment preferably contains Cu at 0.4 at% or more and less than 0.7 at%. More specifically, M f is represented by Cu g M ′ h , where M ′ is one or more elements selected from V, Mn, Co, Ni, and Zn, and 0.4 at% ≦ g <0.7 at% And f = g + h is preferably satisfied. When the M element satisfies the above-described conditions, the rust prevention property and the amorphous forming ability are further improved in the soft magnetic powder. When the ratio of Cu is less than 0.7 at%, a powder having a high ratio of the amorphous phase is obtained, and preferably 0.65 at% or less. Further, if the Cu ratio is 0.4 at% or more, the precipitation amount of αFe nanocrystals is increased and a uniform nanostructure is easily obtained, and if it is 0.5 at% or more, corrosion resistance is remarkably improved and αFe This is more preferable because the amount of deposited nanocrystals is further increased and soft magnetic properties are improved.
　本実施の形態の軟磁性粉末においては、前述のように、Ｃｒの割合はｅ（ａｔ％）である。ここでＣｕの割合は（０．２ｅ－０．１）ａｔ％以上であり、且つ、（２ｅ＋０．５）ａｔ％以下であることが好ましい。また、Ｐの割合は、（６－２ｅ）ａｔ％以上であり、且つ、（２１－５ｅ）ａｔ％以下であることが好ましい。Ｃｕ及びＰの割合をＣｒの割合ｅ（ａｔ％）に対して上記のように設定することにより、本実施の形態の軟磁性粉末において防錆性と軟磁気特性とをより高度に両立することができる。 In the soft magnetic powder of the present embodiment, as described above, the Cr ratio is e (at%). Here, the ratio of Cu is preferably (0.2e−0.1) at% or more and (2e + 0.5) at% or less. Further, the ratio of P is preferably (6-2e) at% or more and (21-5e) at% or less. By setting the proportions of Cu and P to the proportion e (at%) of Cr as described above, the soft magnetic powder of the present embodiment can achieve both rust prevention and soft magnetic properties at a higher level. Can do.
　本実施の形態による軟磁性粉末は、Ｆｅの３ａｔ％以下を、Ｎｂ、Ｚｒ、Ｈｆ、Ｍｏ、Ｔａ、Ｗ、Ａｇ、Ａｕ、Ｐｄ、Ｋ、Ｃａ、Ｍｇ、Ｓｎ、Ｔｉ、Ａｌ、Ｓ、Ｃ、Ｏ、Ｎ、Ｙ及び希土類元素から選ばれる１種類以上の元素と置換してなるものが好ましい。このような元素が含まれることにより、熱処理後の均一なナノ結晶化が容易となる。 In the soft magnetic powder according to the present embodiment, 3 at% or less of Fe, Nb, Zr, Hf, Mo, Ta, W, Ag, Au, Pd, K, Ca, Mg, Sn, Ti, Al, S, C One obtained by substituting one or more elements selected from O, N, Y and rare earth elements is preferable. By including such an element, uniform nanocrystallization after the heat treatment is facilitated.
　本実施の形態の軟磁性粉末に含まれる微量元素のうち、Ａｌ、Ｔｉ、Ｓ、Ｎ、Ｏは、原料や製造工程から混入する微量元素である。従って、軟磁性粉末がこれらの微量元素を様々な含有量で含有する可能性がある。また、これらの微量元素は、製造される軟磁性粉末の軟磁気特性に影響を与えるものである。よって、製造される軟磁性粉末において良好な軟磁気特性を得るためには、軟磁性粉末に含まれるこれらの微量元素の含有量を制御する必要がある。 Among the trace elements contained in the soft magnetic powder of the present embodiment, Al, Ti, S, N, and O are trace elements mixed from raw materials and manufacturing processes. Therefore, the soft magnetic powder may contain these trace elements in various contents. These trace elements affect the soft magnetic properties of the soft magnetic powder produced. Therefore, in order to obtain good soft magnetic characteristics in the produced soft magnetic powder, it is necessary to control the contents of these trace elements contained in the soft magnetic powder.
　上記微量元素において、Ａｌは、Ｆｅ－ＰやＦｅ－Ｂなどの工業原料を用いることにより、製造される軟磁性粉末に混入する微量元素である。Ａｌの軟磁性粉末への混入は非晶質の割合や軟磁気特性の低下を招来する。よって、Ａｌの含有量は、非晶質の割合の低下を避けるため、０．０５質量％以下とすることが好ましく、更なる非晶質の割合の向上と軟磁気特性への影響の抑制のため、０．００５質量％以下とすることがより好ましい。 In the above trace elements, Al is a trace element mixed in the soft magnetic powder produced by using industrial raw materials such as Fe—P and Fe—B. When Al is mixed into the soft magnetic powder, the amorphous ratio and soft magnetic properties are reduced. Therefore, the content of Al is preferably 0.05% by mass or less in order to avoid a decrease in the ratio of amorphous, and further improvement of the ratio of amorphous and suppression of influence on soft magnetic properties are suppressed. Therefore, it is more preferable to set it as 0.005 mass% or less.
　上記微量元素において、Ｔｉは、Ｆｅ－ＰやＦｅ－Ｂなどの工業原料を用いることにより、製造される軟磁性粉末に混入する微量元素である。Ｔｉの軟磁性粉末への混入は非晶質の割合や軟磁気特性の低下を招来する。よって、Ｔｉの含有量は、非晶質の割合の低下を避けるため、０．０５質量％以下にすることが好ましく、更なる非晶質の割合の向上と軟磁気特性への影響の抑制のため、０．００５質量％以下とすることがより好ましい。 In the above trace elements, Ti is a trace element mixed in the soft magnetic powder produced by using industrial raw materials such as Fe-P and Fe-B. Incorporation of Ti into the soft magnetic powder causes a decrease in the amorphous ratio and soft magnetic properties. Therefore, the Ti content is preferably 0.05% by mass or less in order to avoid a decrease in the amorphous ratio, which further improves the amorphous ratio and suppresses the influence on the soft magnetic properties. Therefore, it is more preferable to set it as 0.005 mass% or less.
　上記微量元素において、Ｓは、Ｆｅ－ＰやＦｅ－Ｂなどの工業原料を用いることにより、製造される軟磁性粉末に混入する微量元素である。Ｓの微量添加により軟磁性粉末の球状化を促進する効果がある。しかしながら、Ｓを過剰に添加した場合、不均一なナノ結晶の組織化や軟磁気特性の低下を招来する。よって、Ｓの含有量は、軟磁気特性の低下を避けるため、０．５質量％以下にすることが好ましく、０．０５質量％以下にすることがより好ましい。 In the above trace elements, S is a trace element mixed in the soft magnetic powder produced by using industrial raw materials such as Fe-P and Fe-B. The addition of a small amount of S has the effect of promoting the spheroidization of the soft magnetic powder. However, when S is added excessively, non-uniform nanocrystal organization and soft magnetic properties are reduced. Therefore, the S content is preferably 0.5% by mass or less, and more preferably 0.05% by mass or less in order to avoid a decrease in soft magnetic properties.
　上記微量元素において、Ｎは、工業原料に由来して、あるいは、アトマイズや熱処理時に空気中から軟磁性粉末に混入する微量元素である。Ｎの軟磁性粉末への混入は、軟磁性粉末の非晶質の割合の低下、軟磁性粉末を成形する際の充填率の低下及び軟磁気特性の低下を招来する。よって、Ｎの含有量は、非晶質の割合や軟磁気特性の低下を抑制するため、０．０１質量％以下とすることが好ましく、０．００２質量％以下とすることがより好ましい。 In the above trace elements, N is a trace element derived from industrial raw materials or mixed into the soft magnetic powder from the air during atomization or heat treatment. Incorporation of N into the soft magnetic powder leads to a decrease in the amorphous ratio of the soft magnetic powder, a decrease in filling rate when the soft magnetic powder is formed, and a decrease in soft magnetic characteristics. Therefore, the N content is preferably 0.01% by mass or less, and more preferably 0.002% by mass or less, in order to suppress a decrease in the amorphous ratio and soft magnetic properties.
　上記微量元素において、Ｏは、工業原料に由来して、あるいは、アトマイズ時や乾燥時に空気中から軟磁性粉末に混入する微量元素である。Оの軟磁性粉末への混入は、軟磁性粉末の非晶質の割合の低下、軟磁性粉末を成形する際の充填率の低下及び軟磁気特性の低下を招来する。よって、Ｏの含有量は、非晶質の割合の低下を抑制するため、１．０質量％以下とすることが好ましく、また、軟磁性粉末を成形する際の充填率の低下や軟磁気特性の低下を抑制するため、０．３質量％以下とすることがより好ましい。なお本実施の形態においては、Ｃｒを含む酸化被膜が軟磁性粉末の粉体の表面に形成されているため、微量のＯが軟磁性粉末に意図的に含有されている。また、このような酸化被膜に加えて、軟磁性粉末の表面に樹脂やセラミックなどにより絶縁性被覆を形成することにより、軟磁性粉末間の絶縁性を向上させてもよく、またこれらの酸化被膜及び絶縁性被覆を含めて、Ｏの含有量は１．０質量％を超えてもよい。 In the above trace elements, O is a trace element derived from industrial raw materials, or mixed in the soft magnetic powder from the air during atomization or drying. Incorporation of О into the soft magnetic powder leads to a decrease in the amorphous ratio of the soft magnetic powder, a decrease in the filling rate when the soft magnetic powder is formed, and a decrease in the soft magnetic properties. Therefore, the content of O is preferably set to 1.0% by mass or less in order to suppress a decrease in the ratio of amorphous, and a decrease in filling rate when soft magnetic powder is molded or a soft magnetic property. In order to suppress the decrease in the amount, it is more preferably set to 0.3% by mass or less. In this embodiment, since the oxide film containing Cr is formed on the surface of the soft magnetic powder, a small amount of O is intentionally contained in the soft magnetic powder. In addition to such an oxide film, the insulating property between the soft magnetic powders may be improved by forming an insulating coating on the surface of the soft magnetic powder with resin or ceramic. In addition, the content of O including the insulating coating may exceed 1.0% by mass.
　以下、本実施の形態における軟磁性粉末、圧粉磁芯、磁性部品及びインダクタの磁芯の製造方法を説明しつつ、更に詳しく説明する。 Hereinafter, the method for manufacturing the magnetic core of the soft magnetic powder, the dust core, the magnetic component, and the inductor according to the present embodiment will be described in more detail.
　本実施の形態による軟磁性粉末は、様々な製造方法で作製できる。例えば、軟磁性粉末は、水アトマイズ法やガスアトマイズ法のようなアトマイズ法によって作製してもよい。なお、本実施の形態の軟磁性粉末は、防錆性を付与するＣｒを含有しているため、水を用いた冷却法で作製しても粉体の表面に錆を生じることはない。アトマイズ法による粉末作製工程において、まず、原料を準備する。次に、原料を、所定の組成になるように秤量し、溶解して合金溶湯を作製する。このとき、本実施の形態の軟磁性粉末は、融点が低いため、溶解のための消費電力を削減できる。次に、合金溶湯をノズルから排出して、高圧のガスや水を使用して合金溶滴に分断し、これにより微細な軟磁性粉末を作製する。 The soft magnetic powder according to the present embodiment can be produced by various manufacturing methods. For example, the soft magnetic powder may be produced by an atomizing method such as a water atomizing method or a gas atomizing method. In addition, since the soft magnetic powder of this Embodiment contains Cr which provides rust prevention property, even if it produces with the cooling method using water, it does not produce rust on the surface of powder. In the powder preparation process by the atomizing method, first, raw materials are prepared. Next, the raw materials are weighed so as to have a predetermined composition and melted to produce a molten alloy. At this time, since the soft magnetic powder of the present embodiment has a low melting point, power consumption for dissolution can be reduced. Next, the molten alloy is discharged from the nozzle and divided into alloy droplets using high-pressure gas or water, thereby producing a fine soft magnetic powder.
　上述の粉末作製工程において、分断に使用するガスは、アルゴンや窒素などの不活性ガスであってもよい。また、冷却速度を向上させるため、分断直後の合金溶滴を冷却用の液体や固体に接触させて急冷してもよいし、合金溶滴を再分断して更に微細化してもよい。冷却用に液体を使用する場合、例えば水や油を使用してもよい。冷却用に固体を使用する場合、例えば回転銅ロールや回転アルミ板を使用してもよい。但し、冷却用の液体や固体は、これに限定されず、様々な材料を使用できる。なお、本実施の形態の軟磁性粉末は防錆性を付与するＣｒを含有しているため、量産性に優れた水を用いた冷却法を採用することができる。 In the above-described powder production process, the gas used for cutting may be an inert gas such as argon or nitrogen. Further, in order to improve the cooling rate, the alloy droplets immediately after the division may be brought into contact with a cooling liquid or solid to be rapidly cooled, or the alloy droplets may be redivided and further refined. When using a liquid for cooling, for example, water or oil may be used. When a solid is used for cooling, for example, a rotating copper roll or a rotating aluminum plate may be used. However, the cooling liquid or solid is not limited to this, and various materials can be used. In addition, since the soft magnetic powder of this Embodiment contains Cr which provides rust prevention property, the cooling method using the water excellent in mass-productivity is employable.
　また上述の粉末作製工程において、作製条件を変えることにより、軟磁性粉末の粉末形状及び粒径を調整できる。本実施の形態によれば、合金溶湯の粘性が低いため、軟磁性粉末を球形状に作製しやすい。本実施の形態の軟磁性粉末の平均粒径は、２００μｍ以下であることが好ましく、非晶質化度を向上させるためには１００μｍ以下であることがより好ましい。また、軟磁性粉末の粒度分布が極端に広い場合には、望ましくない粒度偏析を引き起こす原因となり得る。このため、軟磁性粉末の最大粒径は、２００μｍ以下であることが好ましい。また本実施の形態の軟磁性粉末は、非晶質相を９０％以上含んでいることが好ましい。これにより、本実施の形態の軟磁性粉末は、優れた軟磁気特性を有している。加えて本実施の形態の軟磁性粉末は、タップ密度が３．５ｇ／ｃｍ３以上である。これにより、本実施の形態の軟磁性粉末を用いて圧粉磁芯等を作製した場合、充填率を高くすることができる。 Moreover, in the above-mentioned powder production process, the powder shape and particle size of the soft magnetic powder can be adjusted by changing the production conditions. According to this embodiment, since the viscosity of the molten alloy is low, it is easy to produce a soft magnetic powder into a spherical shape. The average particle size of the soft magnetic powder of the present embodiment is preferably 200 μm or less, and more preferably 100 μm or less in order to improve the degree of amorphization. In addition, when the particle size distribution of the soft magnetic powder is extremely wide, it may cause undesirable particle size segregation. For this reason, the maximum particle diameter of the soft magnetic powder is preferably 200 μm or less. Further, the soft magnetic powder of the present embodiment preferably contains 90% or more of an amorphous phase. As a result, the soft magnetic powder of the present embodiment has excellent soft magnetic properties. In addition, the soft magnetic powder of the present embodiment has a tap density of 3.5 g / cm 3 or more. Thereby, when a powder magnetic core etc. are produced using the soft-magnetic powder of this Embodiment, a filling rate can be made high.
　上記の軟磁性粉末の粒径は、レーザー粒度分布計によって評価できる。軟磁性粉末の平均粒径は、評価した粒径から算出できる。軟磁性粉末のＸ線回析結果のピーク位置から、αＦｅ（－Ｓｉ）相、化合物相などの析出相を同定できる。また、タップ密度の試験方法は、規格ＪＩＳ Ｚ２５１２（金属粉－タップ密度測定方法）に従う。 The particle size of the soft magnetic powder can be evaluated by a laser particle size distribution meter. The average particle size of the soft magnetic powder can be calculated from the evaluated particle size. From the peak position of the X-ray diffraction result of the soft magnetic powder, the precipitated phase such as αFe (-Si) phase and compound phase can be identified. The tap density test method follows the standard JIS Z2512 (metal powder-tap density measurement method).
　また上述の粉末作製工程から作製された軟磁性粉末を、前述のように熱処理した場合、αＦｅのナノ結晶が軟磁性粉末中に析出するため、ナノ結晶を含む軟磁性粉末を作製することができる。なお、この熱処理は、前述のように、化合物相を析出させないように、第２結晶化開始温度（Ｔｘ２）以下で行う必要がある。また、この熱処理は、アルゴンや窒素などの不活性雰囲気中において３００℃以上の温度下で行うことが好ましい。但し、軟磁性粉末の表面に酸化層を形成して耐食性や絶縁性を向上させるため、部分的に酸化雰囲気中で熱処理してもよい。また、軟磁性粉末の表面状態を改善するため、部分的に還元雰囲気中で熱処理してもよい。 In addition, when the soft magnetic powder produced from the above-described powder production process is heat-treated as described above, αFe nanocrystals are precipitated in the soft magnetic powder, so that a soft magnetic powder containing nanocrystals can be produced. . In addition, as above-mentioned, it is necessary to perform this heat processing below 2nd crystallization start temperature (Tx2) so that a compound phase may not precipitate. This heat treatment is preferably performed at a temperature of 300 ° C. or higher in an inert atmosphere such as argon or nitrogen. However, in order to improve the corrosion resistance and insulation by forming an oxide layer on the surface of the soft magnetic powder, it may be partially heat-treated in an oxidizing atmosphere. Further, in order to improve the surface state of the soft magnetic powder, it may be partially heat-treated in a reducing atmosphere.
　上記の熱処理により軟磁性粉末中に析出したαＦｅのナノ結晶の平均粒径が５０ｎｍを超えると、結晶磁気異方性が大きくなり軟磁気特性が劣化する。また、αＦｅのナノ結晶の平均粒径が４０ｎｍを超えると、軟磁気特性が多少低下する。従って、αＦｅのナノ結晶の平均粒径は、５０ｎｍ以下であることが好ましく、４０ｎｍ以下であることがより好ましい。 When the average particle diameter of the αFe nanocrystals precipitated in the soft magnetic powder by the heat treatment exceeds 50 nm, the magnetocrystalline anisotropy increases and the soft magnetic properties deteriorate. Further, when the average particle diameter of the αFe nanocrystal exceeds 40 nm, the soft magnetic characteristics are somewhat deteriorated. Accordingly, the average particle diameter of the αFe nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
　また上記の熱処理により軟磁性粉末中に析出したαＦｅのナノ結晶の結晶化度が３５％以上の場合、飽和磁束密度Ｂｓが１．６Ｔ以上に向上する。従って、αＦｅのナノ結晶の結晶化度は、３５％以上であることが好ましい。更に、上記の熱処理により軟磁性粉末中に析出したαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、軟磁気特性の低下の抑制の観点から、７％以下が好ましく、５％以下がより好ましく、３％以下が更に好ましい。 When the crystallinity of the αFe nanocrystals precipitated in the soft magnetic powder by the heat treatment is 35% or more, the saturation magnetic flux density Bs is improved to 1.6 T or more. Therefore, the crystallinity of αFe nanocrystals is preferably 35% or more. Further, the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals precipitated in the soft magnetic powder by the heat treatment is preferably 7% or less, preferably 5% or less, from the viewpoint of suppressing the decrease in soft magnetic properties. Is more preferable, and 3% or less is still more preferable.
　上記のαＦｅのナノ結晶の平均粒径及び結晶化度、並びにαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、Ｘ線回析（ＸＲＤ：X‐ray diffraction）による測定結果をＷＰＰＤ法（Whole-powder-pattern decomposition method）によって解析することで算出できる。また、飽和磁束密度Ｂｓは、振動試料型磁力計（ＶＳＭ：Vibrating Sample Magnetometer）を使用して測定された飽和磁化と、密度から算出できる。 The average particle diameter and crystallinity of the above-mentioned αFe nanocrystals, and the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals were measured by X-ray diffraction (XRD: X-ray diffraction). It can be calculated by analyzing by the method (Whole-powder-pattern decomposition method). The saturation magnetic flux density Bs can be calculated from the saturation magnetization measured using a vibrating sample magnetometer (VSM) and the density.
　上述の粉末作製工程から作製された軟磁性粉末を使用して、圧粉磁芯を製造することができる。例えば、軟磁性粉末を所定の形状に成型した後に所定の熱処理条件による熱処理を施すことで、圧粉磁芯を製造できる。また、この圧粉磁芯を使用して、トランス、インダクタ、モーターや発電機などの磁性部品を製造することができる。以下、軟磁性粉末を使用した本実施の形態の圧粉磁芯の製造方法について説明する。 A powder magnetic core can be manufactured using the soft magnetic powder produced from the above-mentioned powder production process. For example, the powder magnetic core can be manufactured by forming a soft magnetic powder into a predetermined shape and then performing heat treatment under predetermined heat treatment conditions. Moreover, magnetic parts, such as a transformer, an inductor, a motor, and a generator, can be manufactured using this powder magnetic core. Hereinafter, the manufacturing method of the powder magnetic core of this Embodiment using soft magnetic powder is demonstrated.
　本実施の形態の圧粉磁芯の製造方法は、本実施の形態の軟磁性粉末と結合剤との混合物を製造する工程と、この混合物を加圧成型して成型体を製造する工程と、この成型体を熱処理する工程とを備えている。 The method for producing a dust core according to the present embodiment includes a step of producing a mixture of the soft magnetic powder and a binder according to the present embodiment, a step of producing a molded body by press molding the mixture, And a step of heat-treating the molded body.
　まず軟磁性粉末と結合剤との混合物を製造する工程として、本実施の形態の軟磁性粉末を、樹脂等の絶縁性が良好な結合剤と混合して混合物（造粒粉）を得る。ここで結合剤として樹脂を使用する場合、例えば、シリコーン、エポキシ、フェノール、メラミン、ポリウレタン、ポリイミド、ポリアミドイミドを使用してもよい。絶縁性や結着性を向上させるために、樹脂に代えて、又は、樹脂と共に、リン酸塩、ホウ酸塩、クロム酸塩、酸化物(シリカ、アルミナ、マグネシア等)、無機高分子(ポリシラン、ポリゲルマン、ポリスタナン、ポリシロキサン、ポリシルセスキオキサン、ポリシラザン、ポリボラジレン、ポリホスファゼンなど)などの材料を結合剤として使用してもよい。また、複数の結合剤を併用しても良く、異なる結合剤によって２層またはそれ以上の多層構造の被覆を形成しても良い。なお、圧粉磁芯の製造においては、上述のように成型体を熱処理する工程を有していることから、耐熱性の高い結合剤を使用することが好ましい。結合剤の量は、一般的には、０．１～１０質量％程度が好ましく、絶縁性及び充填率を考慮すると、０．３～６質量％程度が好ましい。但し、結合剤の量は、粉末粒径、適用周波数、用途等を考慮して適切に決定すればよい。 First, as a process for producing a mixture of soft magnetic powder and a binder, the soft magnetic powder of the present embodiment is mixed with a binder having good insulating properties such as a resin to obtain a mixture (granulated powder). Here, when a resin is used as the binder, for example, silicone, epoxy, phenol, melamine, polyurethane, polyimide, or polyamideimide may be used. In order to improve insulation and binding properties, phosphate, borate, chromate, oxide (silica, alumina, magnesia, etc.), inorganic polymer (polysilane) instead of or together with resin , Polygermane, polystannane, polysiloxane, polysilsesquioxane, polysilazane, polyborazirene, polyphosphazene, and the like) may be used as the binder. A plurality of binders may be used in combination, and a coating having a multilayer structure of two layers or more may be formed by different binders. In the production of the dust core, it is preferable to use a binder having high heat resistance because it includes a step of heat-treating the molded body as described above. In general, the amount of the binder is preferably about 0.1 to 10% by mass, and is preferably about 0.3 to 6% by mass in consideration of insulation and filling rate. However, the amount of the binder may be appropriately determined in consideration of the powder particle size, application frequency, usage, and the like.
　次に、混合物を加圧成型して成型体を製造する工程として、造粒粉を金型を使用して加圧成型して成型体を得る。ここで造粒粉を加圧成型する際、充填率を向上させると共にナノ結晶化における発熱を抑制するため、本実施の形態による軟磁性粉末よりも軟質のＦｅ、ＦｅＳｉ、ＦｅＳｉＣｒ、ＦｅＳｉＡｌ、ＦｅＮｉ、カルボニル鉄粉等の粉末を１種類以上混ぜてもよい。また、上記の軟質粉末に代えて、又は、上記の軟質粉末と共に、本実施の形態による軟磁性粉末とは粒径の異なる任意の軟磁性粉末を混ぜても良い。このとき、上記粉末の本実施の形態による軟磁性粉末に対する混合比は、７５質量％以下であることが好ましい。 Next, as a step of producing a molded body by pressure molding the mixture, the molded powder is obtained by pressure molding the granulated powder using a mold. Here, when press-molding the granulated powder, Fe, FeSi, FeSiCr, FeSiAl, FeNi, softer than the soft magnetic powder according to the present embodiment, in order to improve the filling rate and suppress heat generation in nanocrystallization. One or more kinds of powders such as carbonyl iron powder may be mixed. Further, instead of the soft powder, or together with the soft powder, any soft magnetic powder having a particle diameter different from that of the soft magnetic powder according to the present embodiment may be mixed. At this time, the mixing ratio of the powder to the soft magnetic powder according to the present embodiment is preferably 75% by mass or less.
　その後、成型体に所定の熱処理条件による熱処理を施す。この熱処理により、軟磁性粉末中にαＦｅのナノ結晶が析出する。この熱処理は、上述の軟磁性粉末に対する熱処理と同様であり、第２結晶化開始温度（Ｔｘ２）以下で行う必要がある。また、この熱処理は、アルゴンや窒素などの不活性雰囲気中において３００℃以上の温度下で行うことが好ましい。但し、成型体の表面に酸化層を形成して耐食性や絶縁性を向上させるため、部分的に酸化雰囲気中で熱処理してもよい。また、成型体の表面状態を改善するため、部分的に還元雰囲気中で熱処理してもよい。 Thereafter, the molded body is subjected to heat treatment under predetermined heat treatment conditions. By this heat treatment, αFe nanocrystals are precipitated in the soft magnetic powder. This heat treatment is the same as the heat treatment for the soft magnetic powder described above, and it is necessary to perform the heat treatment at or below the second crystallization start temperature (Tx2). This heat treatment is preferably performed at a temperature of 300 ° C. or higher in an inert atmosphere such as argon or nitrogen. However, in order to improve the corrosion resistance and insulation by forming an oxide layer on the surface of the molded body, it may be partially heat-treated in an oxidizing atmosphere. Moreover, in order to improve the surface state of a molded object, you may heat-process partially in a reducing atmosphere.
　上述の熱処理により圧粉磁芯を構成する軟磁性粉末中に析出したαＦｅのナノ結晶の平均粒径が５０ｎｍを超えると、結晶磁気異方性が大きくなり軟磁気特性が劣化する。また、αＦｅのナノ結晶の平均粒径が４０ｎｍを超えると、軟磁気特性が多少低下する。従って、αＦｅのナノ結晶の平均粒径は、５０ｎｍ以下であることが好ましく、４０ｎｍ以下であることがより好ましい。 When the average particle diameter of the αFe nanocrystals precipitated in the soft magnetic powder constituting the dust core by the heat treatment described above exceeds 50 nm, the magnetocrystalline anisotropy increases and the soft magnetic properties deteriorate. Further, when the average particle diameter of the αFe nanocrystal exceeds 40 nm, the soft magnetic characteristics are somewhat deteriorated. Accordingly, the average particle diameter of the αFe nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
　上述の熱処理により圧粉磁芯を構成する軟磁性粉末中に析出したαＦｅのナノ結晶の結晶化度が３５％以上の場合、圧粉磁芯の飽和磁束密度が向上し、磁歪が低減できる。また、上述の熱処理により圧粉磁芯を構成する軟磁性粉末中に析出したαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、圧粉磁芯のコアロス低減の観点から、７％以下が好ましく、５％以下がより好ましく、３％以下が更に好ましい。 When the crystallinity of the αFe nanocrystals precipitated in the soft magnetic powder constituting the powder magnetic core by the heat treatment described above is 35% or more, the saturation magnetic flux density of the powder magnetic core is improved and the magnetostriction can be reduced. Further, the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals precipitated in the soft magnetic powder constituting the powder magnetic core by the above heat treatment is 7% from the viewpoint of reducing the core loss of the powder magnetic core. The following is preferable, 5% or less is more preferable, and 3% or less is still more preferable.
　上記のαＦｅのナノ結晶の平均粒径及び結晶化度、並びにαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、Ｘ線回析（ＸＲＤ：X‐ray diffraction）による測定結果をＷＰＰＤ法（Whole-powder-pattern decomposition method）によって解析することで算出できる。 The average particle diameter and crystallinity of the above-mentioned αFe nanocrystals, and the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals were measured by X-ray diffraction (XRD: X-ray diffraction). It can be calculated by analyzing by the method (Whole-powder-pattern decomposition method).
　本実施の形態における圧粉磁芯は、熱処理していない軟磁性粉末を原料として製造されているが、本発明はこれに限定されず、予め熱処理してαＦｅのナノ結晶を析出させた軟磁性粉末を原料として圧粉磁芯を製造してもよい。この場合、上述の圧粉磁芯の製造工程と同様に、造粒および加圧成型を行うことで圧粉磁芯を製造することができる。 The dust core in the present embodiment is manufactured using soft magnetic powder that has not been heat-treated as a raw material. However, the present invention is not limited to this, and soft magnetism in which αFe nanocrystals are deposited in advance by heat treatment. You may manufacture a powder magnetic core from powder. In this case, a dust core can be manufactured by granulating and press-molding similarly to the manufacturing process of the above-mentioned dust core.
　上述の粉末作製工程から作製された軟磁性粉末を使用して、インダクタの磁芯を製造することもできる。以下、軟磁性粉末を使用した本実施の形態のインダクタの磁芯の製造方法について説明する。 The magnetic core of the inductor can also be manufactured using the soft magnetic powder produced from the above-mentioned powder production process. Hereinafter, a method of manufacturing the inductor magnetic core according to the present embodiment using soft magnetic powder will be described.
　本実施の形態のインダクタの磁芯の製造方法は、本実施の形態の軟磁性粉末と結合剤との混合物を製造する工程と、この混合物とコイルとを一体で加圧成型して成型体を製造する工程と、この成型体を熱処理する工程とを備えている。 The inductor magnetic core manufacturing method according to the present embodiment includes a step of manufacturing the mixture of the soft magnetic powder and the binder according to the present embodiment, and press-molding the mixture and the coil together to form a molded body. The manufacturing process and the process of heat-processing this molded object are provided.
　本実施の形態の軟磁性粉末と結合剤との混合物を製造する工程は、上述の圧粉磁芯の製造方法と同様であり、詳細な説明は省略する。 The process for producing the mixture of the soft magnetic powder and the binder according to the present embodiment is the same as the above-described method for producing a dust core, and detailed description thereof is omitted.
　混合物とコイルとを一体で加圧成型して成型体を製造する工程としては、予め金型内にコイルを設置した後、混合物（造粒粉）を金型に入れて、混合物（造粒粉）とコイルとを一体で加圧成型して成型体を得る。ここで混合物（造粒紛）とコイルとを一体で加圧成型する際、充填率を向上させると共にナノ結晶化における発熱を抑制するため、本実施の形態による軟磁性粉末よりも軟質のＦｅ、ＦｅＳｉ、ＦｅＳｉＣｒ、ＦｅＳｉＡｌ、ＦｅＮｉ、カルボニル鉄粉等の粉末を１種類以上混ぜてもよい。また、上記の軟質粉末に代えて、又は、上記の軟質粉末と共に、本実施の形態による軟磁性粉末とは粒径の異なる任意の軟磁性粉末を混ぜても良い。このとき、上記粉末の本実施の形態による軟磁性粉末に対する混合比は、７５質量％以下であることが好ましい。 As a process for producing a molded body by integrally pressure-molding the mixture and the coil, after placing the coil in the mold in advance, the mixture (granulated powder) is put into the mold and the mixture (granulated powder) ) And the coil are integrally pressure-molded to obtain a molded body. Here, when the mixture (granulated powder) and the coil are integrally pressure-molded, in order to improve the filling rate and suppress heat generation in nanocrystallization, Fe that is softer than the soft magnetic powder according to the present embodiment, One or more kinds of powders such as FeSi, FeSiCr, FeSiAl, FeNi, and carbonyl iron powder may be mixed. Further, instead of the soft powder, or together with the soft powder, any soft magnetic powder having a particle diameter different from that of the soft magnetic powder according to the present embodiment may be mixed. At this time, the mixing ratio of the powder to the soft magnetic powder according to the present embodiment is preferably 75% by mass or less.
　成型体を熱処理する工程についても、上述の圧粉磁芯の製造方法と同様であり、詳細な説明は省略する。 The process of heat-treating the molded body is also the same as the above-described method for manufacturing a dust core, and detailed description thereof is omitted.
　上述の熱処理によりインダクタの磁芯を構成する軟磁性粉末中に析出したαＦｅのナノ結晶の平均粒径が５０ｎｍを超えると、結晶磁気異方性が大きくなり軟磁気特性が劣化する。また、αＦｅのナノ結晶の平均粒径が４０ｎｍを超えると、軟磁気特性が多少低下する。従って、αＦｅのナノ結晶の平均粒径は、５０ｎｍ以下であることが好ましく、４０ｎｍ以下であることがより好ましい。 When the average particle diameter of the αFe nanocrystals precipitated in the soft magnetic powder constituting the magnetic core of the inductor by the above heat treatment exceeds 50 nm, the magnetocrystalline anisotropy increases and the soft magnetic properties deteriorate. Further, when the average particle diameter of the αFe nanocrystal exceeds 40 nm, the soft magnetic characteristics are somewhat deteriorated. Accordingly, the average particle diameter of the αFe nanocrystals is preferably 50 nm or less, and more preferably 40 nm or less.
　上述の熱処理によりインダクタの磁芯を構成する軟磁性粉末中に析出したαＦｅのナノ結晶の結晶化度が３５％以上の場合、圧粉磁芯の飽和磁束密度が向上し、磁歪が低減できる。また、上述の熱処理によりインダクタの磁芯を構成する軟磁性粉末中に析出したαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、インダクタの磁芯のコアロス低減の観点から、７％以下が好ましく、５％以下がより好ましく、３％以下が更に好ましい。 When the crystallinity of the αFe nanocrystals deposited in the soft magnetic powder constituting the magnetic core of the inductor by the above heat treatment is 35% or more, the saturation magnetic flux density of the powder magnetic core is improved and the magnetostriction can be reduced. Further, the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals precipitated in the soft magnetic powder constituting the magnetic core of the inductor by the heat treatment described above is 7% from the viewpoint of reducing the core loss of the magnetic core of the inductor. The following is preferable, 5% or less is more preferable, and 3% or less is still more preferable.
　上記のαＦｅのナノ結晶の平均粒径及び結晶化度、並びにαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、上述の圧粉磁芯の場合と同様に測定することができる。 The average particle size and crystallinity of the αFe nanocrystals and the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals can be measured in the same manner as in the case of the above-described dust core.
　本実施の形態におけるインダクタの磁芯は、熱処理していない軟磁性粉末を原料として製造されているが、本発明はこれに限定されず、予め熱処理してαＦｅのナノ結晶を析出させた軟磁性粉末を原料としてインダクタの磁芯を製造してもよい。この場合、上述のインダクタの磁芯の製造工程と同様に、造粒および加圧成型を行うことでインダクタの磁芯を製造することができる。 The inductor magnetic core in this embodiment is manufactured using soft magnetic powder that has not been heat-treated as a raw material. However, the present invention is not limited to this, and soft magnetism in which αFe nanocrystals are deposited in advance by heat treatment. The magnetic core of the inductor may be manufactured using powder as a raw material. In this case, the inductor magnetic core can be manufactured by granulation and pressure molding in the same manner as the above-described inductor magnetic core manufacturing process.
　以上のように作製した本実施の形態の圧粉磁芯及びインダクタの磁芯には、作製工程に係らず、本実施の形態の軟磁性粉末が用いられている。同様に、本実施の形態の磁性部品には、本実施の形態の軟磁性粉末が用いられている。 The soft magnetic powder of the present embodiment is used for the dust core and the inductor core of the present embodiment manufactured as described above regardless of the manufacturing process. Similarly, the soft magnetic powder of this embodiment is used for the magnetic component of this embodiment.
　以下、本発明の実施の形態について、複数の実施例を参照しながら更に詳細に説明する。 Hereinafter, embodiments of the present invention will be described in more detail with reference to a plurality of examples.
　（実施例１～１２及び比較例１～８）
　下記の表１に記載の実施例１～１２及び比較例１～８の軟磁性粉末の原料として、工業純鉄、フェロシリコン、フェロリン、フェロボロン、及び電解銅を準備した。原料を表１に記載の実施例１～１２及び比較例１～８の合金組成となるように秤量し、アルゴン雰囲気中で高周波溶解によって溶解して合金溶湯を作製した。次に、作製された合金溶湯をガスアトマイズした後、冷却水により急冷して、平均粒径５０μｍの軟磁性粉末を作製した。作製された軟磁性粉末の表面に生じた錆の状態を外観観察した。作製された軟磁性粉末の析出相をＸ線回析（ＸＲＤ：X‐ray diffraction）によって評価して非晶質相の割合を算出した。また、作製された軟磁性粉末を、電気炉にてアルゴン雰囲気中で表１に示す熱処理温度にて熱処理を行った。熱処理された軟磁性粉末について振動試料型磁力計（ＶＳＭ）で飽和磁束密度Ｂｓを測定した。作製された軟磁性粉末の測定及び評価の結果を表１に示す。 (Examples 1 to 12 and Comparative Examples 1 to 8)
Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 1 to 12 and Comparative Examples 1 to 8 shown in Table 1 below. The raw materials were weighed so as to have the alloy compositions of Examples 1 to 12 and Comparative Examples 1 to 8 shown in Table 1, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 μm. The appearance of rust generated on the surface of the produced soft magnetic powder was observed. The deposited phase of the produced soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase. Moreover, the produced soft magnetic powder was heat-treated in an electric furnace at a heat treatment temperature shown in Table 1 in an argon atmosphere. The saturation magnetic flux density Bs of the heat-treated soft magnetic powder was measured with a vibrating sample magnetometer (VSM). Table 1 shows the results of measurement and evaluation of the produced soft magnetic powder.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　表１に示されるように、Ｃｒを含まない比較例１においては、非晶質相が４２％と低く、また表面に錆の発生が確認された。またＣｒを含まないＦｅアモルファスである比較例７においても、表面に錆の発生が認められた。比較例５はＣｒを含んでいるが、非晶質相が８４％と低かった。また、比較例４はＣｒを含んでいるが、非晶質相が６４％と低く、錆の発生を抑制できなかった。一方、実施例１～１２においては、非晶質相が９６～１００％であった。即ち、実施例１～１２の全ての非晶質相は、９０％以上であった。また実施例１～１２において、表面に錆の発生も認められなかった。比較例３、５、７及び８においては、飽和磁束密度Ｂｓが、１．３２～１．５５Ｔであった。即ち、比較例３、５、７及び８の全ての飽和磁束密度Ｂｓが、１．５５Ｔ以下であった。一方、実施例１～１２においては、飽和磁束密度Ｂｓは、１．５６～１．７２Ｔであった。即ち、実施例１～１２の全ての飽和磁束密度Ｂｓは、１．５６Ｔ以上であった。 As shown in Table 1, in Comparative Example 1 containing no Cr, the amorphous phase was as low as 42%, and the occurrence of rust on the surface was confirmed. Further, in Comparative Example 7 which is Fe amorphous not containing Cr, generation of rust was observed on the surface. Comparative Example 5 contained Cr, but the amorphous phase was as low as 84%. Moreover, although the comparative example 4 contained Cr, the amorphous phase was as low as 64%, and generation | occurrence | production of rust was not able to be suppressed. On the other hand, in Examples 1 to 12, the amorphous phase was 96 to 100%. That is, all the amorphous phases of Examples 1 to 12 were 90% or more. In Examples 1 to 12, no rust was observed on the surface. In Comparative Examples 3, 5, 7, and 8, the saturation magnetic flux density Bs was 1.32 to 1.55T. That is, all the saturation magnetic flux densities Bs of Comparative Examples 3, 5, 7, and 8 were 1.55 T or less. On the other hand, in Examples 1 to 12, the saturation magnetic flux density Bs was 1.56 to 1.72T. That is, all the saturation magnetic flux densities Bs of Examples 1 to 12 were 1.56 T or more.
　実施例１～１２及び比較例１～８の軟磁性粉末から圧粉磁芯を作製した。詳しくは、上述の方法で作製された軟磁性粉末を、２質量％のシリコーン樹脂を使用して造粒し、外径１３ｍｍ且つ内径８ｍｍの金型を使用して１０ｔｏｎ／ｃｍ２の成型圧力によって成型し硬化処理を施した。その後、電気炉にてアルゴン雰囲気中で表１に示す熱処理温度にて熱処理を行い、圧粉磁芯を作製した。得られた圧粉磁芯について、交流ＢＨアナライザーを使用して２０ｋＨｚ－１００ｍＴのコアロスを測定した。また、得られた圧粉磁芯について、６０℃-９０％ＲＨにおける恒温恒湿試験を実施し、外観観察にて腐食状況を確認した。加えて、得られた圧粉磁芯の表面をＸＲＤ測定してＷＰＰＤ法で解析することにより、圧粉磁芯に含まれる軟磁性粉末中のαＦｅのナノ結晶の平均粒径と結晶化度を算出した。作製された圧粉磁芯の測定及び評価の結果を表２に示す。また、実施例６、７及び８の圧粉磁芯の作製に使用した軟磁性粉末についてＤＳＣ分析を行い、得られたＤＳＣ曲線からΔＴを算出した。 Powder magnetic cores were produced from the soft magnetic powders of Examples 1 to 12 and Comparative Examples 1 to 8. Specifically, the soft magnetic powder produced by the above-described method is granulated using 2% by mass of silicone resin, and a mold having an outer diameter of 13 mm and an inner diameter of 8 mm is used with a molding pressure of 10 ton / cm 2 . Molded and cured. Then, it heat-processed with the heat processing temperature shown in Table 1 in argon atmosphere with the electric furnace, and produced the dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. Further, the obtained dust core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. In addition, by measuring the surface of the obtained dust core by XRD and analyzing it by the WPPD method, the average particle diameter and crystallinity of the αFe nanocrystals in the soft magnetic powder contained in the dust core are determined. Calculated. Table 2 shows the results of measurement and evaluation of the produced dust core. Moreover, DSC analysis was performed about the soft magnetic powder used for preparation of the powder magnetic cores of Examples 6, 7 and 8, and ΔT was calculated from the obtained DSC curve.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
　表２に示されるように、比較例１～８のコアロスは、７５～１４５０ｋＷ／ｍ３であった。一方、実施例１～１２のコアロスは、７０～１６０ｋＷ／ｍ３であった。即ち、実施例１～１２の全てのコアロスは、低い値であった。また恒温恒湿試験においては、比較例１、２及び７において腐食が確認されたが、実施例１～１２の全てにおいて腐食は確認されなかった。 As shown in Table 2, the core loss of Comparative Examples 1 to 8 was 75 to 1450 kW / m 3 . On the other hand, the core loss of Examples 1 to 12 was 70 to 160 kW / m 3 . That is, all core losses in Examples 1 to 12 were low values. In the constant temperature and humidity test, corrosion was confirmed in Comparative Examples 1, 2, and 7, but corrosion was not confirmed in all of Examples 1 to 12.
　上記の測定及び評価の結果から、軟磁性粉末中のＦｅの割合は、比較例１と比較例２とを非晶質相及び錆の発生の観点から比較すると、８５ａｔ％以下が好ましいことが理解される。軟磁性粉末中のＦｅの割合は、比較例２と実施例１とを非晶質相及び錆の発生の観点から比較すると、８３．５ａｔ％以下がより好ましいことが理解される。また、軟磁性粉末中のＦｅの割合は、実施例５と比較例３とを飽和磁束密度Ｂｓの観点から比較すると、７８ａｔ％以上が好ましいことが理解される。軟磁性粉末中のＦｅの割合は、実施例４と実施例５とを飽和磁束密度Ｂｓの観点から比較すると、７９ａｔ％以上がより好ましいことが理解される。軟磁性粉末中のＦｅの割合は、実施例１１と実施例１２とを飽和磁束密度Ｂｓの観点から比較すると、８０．５ａｔ％以上が更に好ましいことが理解される。 From the results of the above measurements and evaluations, it is understood that the proportion of Fe in the soft magnetic powder is preferably 85 at% or less when comparing Comparative Example 1 and Comparative Example 2 from the viewpoint of generation of an amorphous phase and rust. Is done. It is understood that the ratio of Fe in the soft magnetic powder is more preferably 83.5 at% or less when Comparative Example 2 and Example 1 are compared from the viewpoint of the generation of an amorphous phase and rust. Further, it is understood that the ratio of Fe in the soft magnetic powder is preferably 78 at% or more when Example 5 and Comparative Example 3 are compared from the viewpoint of saturation magnetic flux density Bs. It is understood that the Fe ratio in the soft magnetic powder is more preferably 79 at% or more when Example 4 and Example 5 are compared from the viewpoint of the saturation magnetic flux density Bs. It is understood that the Fe ratio in the soft magnetic powder is more preferably 80.5 at% or more when Example 11 and Example 12 are compared from the viewpoint of the saturation magnetic flux density Bs.
　また上記の測定及び評価の結果から、軟磁性粉末中のＳｉの割合は、実施例６と実施例７とをコアロスの観点から比較すると、０．１ａｔ％以上が好ましいことが理解される。また、軟磁性粉末中のＳｉの割合は、実施例９と比較例４とをコアロスの観点から比較すると、６ａｔ％以下が好ましいことが理解される。 Further, from the results of the above measurements and evaluations, it is understood that the Si ratio in the soft magnetic powder is preferably 0.1 at% or more when Example 6 and Example 7 are compared from the viewpoint of core loss. Further, it is understood that the Si ratio in the soft magnetic powder is preferably 6 at% or less when Example 9 and Comparative Example 4 are compared from the viewpoint of core loss.
　上述のＤＳＣ分析から、実施例６、７及び８の圧粉磁芯の作製に使用した軟磁性粉末のΔＴは、夫々、８９℃、９３℃及び１０５℃と算出された。この結果から、Ｓｉの割合の増加に伴ってΔＴが増大することが理解される。特に、１０ｇ程度以上の大型コアを成型する場合には、ΔＴが１００℃以上となることが好ましいため、Ｓｉの割合としては２ａｔ％以上がより好ましいことが理解される。 From the above-mentioned DSC analysis, ΔT of the soft magnetic powder used for producing the dust cores of Examples 6, 7 and 8 was calculated as 89 ° C., 93 ° C. and 105 ° C., respectively. From this result, it is understood that ΔT increases as the proportion of Si increases. In particular, when molding a large core of about 10 g or more, it is understood that ΔT is preferably 100 ° C. or more, and therefore the Si ratio is more preferably 2 at% or more.
　また上記の測定及び評価の結果から、軟磁性粉末中のＢの割合は、比較例１と比較例２とを非晶質相およびコアロスの観点から比較すると、１０ａｔ％以下が好ましいことが理解される。また、軟磁性粉末中のＢの割合は、実施例１０と比較例５とを非晶質相およびコアロスの観点から比較すると、４ａｔ％以上が好ましいことが理解される。 Further, from the results of the above measurements and evaluations, it is understood that the ratio of B in the soft magnetic powder is preferably 10 at% or less when comparing Comparative Example 1 and Comparative Example 2 from the viewpoint of the amorphous phase and core loss. The Further, it is understood that the ratio of B in the soft magnetic powder is preferably 4 at% or more when Example 10 and Comparative Example 5 are compared from the viewpoint of the amorphous phase and the core loss.
　加えて、上記の測定及び評価の結果から、軟磁性粉末中のＰの割合は、実施例１０、比較例５、比較例７と比較例８とを飽和磁束密度Ｂｓの観点から比較すると、１２ａｔ％以下が好ましいことが理解される。軟磁性粉末中のＰの割合は、実施例６、実施例１０と比較例６とを飽和磁束密度Ｂｓの観点から比較すると、１０ａｔ％以下がより好ましいことが理解される。軟磁性粉末中のＰの割合は、実施例５と比較例３とを飽和磁束密度Ｂｓの観点から比較すると、８ａｔ％以下がより好ましいことが理解される。また、軟磁性粉末中のＰの割合は、比較例２と実施例３とをコアロスの観点から比較すると、５ａｔ％以上であることが好ましいことが理解される。また軟磁性粉末中のＰの割合は、比較例２、実施例１、比較例７と比較例８とをコアロス及び恒温恒湿試験の観点から比較すると、６ａｔ％を超えることがより好ましいことが理解される。また、軟磁性粉末中のＰの割合は、実施例８と実施例９とを非晶質相及びコアロスの観点から比較すると、８ａｔ％を超えることが更に好ましいことが理解される。 In addition, from the results of the above measurement and evaluation, the proportion of P in the soft magnetic powder is 12 ata when comparing Example 10, Comparative Example 5, Comparative Example 7, and Comparative Example 8 from the viewpoint of saturation magnetic flux density Bs. % Is preferred. It is understood that the ratio of P in the soft magnetic powder is more preferably 10 at% or less when Example 6, Example 10 and Comparative Example 6 are compared from the viewpoint of saturation magnetic flux density Bs. When the ratio of P in the soft magnetic powder is compared between Example 5 and Comparative Example 3 from the viewpoint of the saturation magnetic flux density Bs, it is understood that 8 at% or less is more preferable. Further, it is understood that the proportion of P in the soft magnetic powder is preferably 5 at% or more when comparing Comparative Example 2 and Example 3 from the viewpoint of core loss. Further, it is more preferable that the ratio of P in the soft magnetic powder exceeds 6 at% when comparing Comparative Example 2, Example 1, Comparative Example 7 and Comparative Example 8 from the viewpoint of core loss and constant temperature and humidity test. Understood. Further, it is understood that the ratio of P in the soft magnetic powder is more preferably more than 8 at% when comparing Example 8 and Example 9 from the viewpoint of the amorphous phase and the core loss.
　実施例１の圧粉磁芯において、析出したαＦｅのナノ結晶の平均粒径は３６ｎｍと算出され、析出したαＦｅのナノ結晶の結晶化度は５１％と算出された。また、実施例２の圧粉磁芯において、析出したαＦｅのナノ結晶の平均粒径は２９ｎｍと算出され、析出したαＦｅのナノ結晶の結晶化度は４６％と算出された。これにより、実施例１及び実施例２の圧粉磁芯中の軟磁性粉末において、平均粒径が４０ｎｍ以下であって結晶化度３５％以上であるαＦｅのナノ組織が形成されていることが確認された。 In the dust core of Example 1, the average particle diameter of the precipitated αFe nanocrystals was calculated to be 36 nm, and the crystallinity of the precipitated αFe nanocrystals was calculated to be 51%. In the dust core of Example 2, the average particle diameter of the precipitated αFe nanocrystals was calculated to be 29 nm, and the crystallinity of the precipitated αFe nanocrystals was calculated to be 46%. Thereby, in the soft magnetic powder in the dust cores of Example 1 and Example 2, an αFe nanostructure having an average particle diameter of 40 nm or less and a crystallinity of 35% or more is formed. confirmed.
　（実施例１３～２５及び比較例９、１０）
　下記の表３に記載の実施例１３～２５及び比較例９、１０の軟磁性粉末の原料として、工業純鉄、フェロシリコン、フェロリン、フェロボロン、及び電解銅を準備した。原料を表３に記載の実施例１３～２５及び比較例９、１０の合金組成となるように秤量し、アルゴン雰囲気中で高周波溶解によって溶解して合金溶湯を作製した。次に、作製された合金溶湯をガスアトマイズした後、冷却水により急冷して、平均粒径５０μｍの軟磁性粉末を作製した。作製された軟磁性粉末の表面に生じた錆の状態を外観観察した。作製された軟磁性粉末の析出相をＸ線回析（ＸＲＤ：X‐ray diffraction）によって評価して非晶質相の割合を算出した。また、作製された軟磁性粉末を電気炉にてアルゴン雰囲気中で表３に示す熱処理温度にて熱処理を行った。熱処理された軟磁性粉末について振動試料型磁力計（ＶＳＭ）で飽和磁束密度Ｂｓを測定した。作製された軟磁性粉末の測定及び評価の結果を表３に示す。 (Examples 13 to 25 and Comparative Examples 9 and 10)
Industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powders of Examples 13 to 25 and Comparative Examples 9 and 10 shown in Table 3 below. The raw materials were weighed so as to have the alloy compositions of Examples 13 to 25 and Comparative Examples 9 and 10 shown in Table 3, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 μm. The appearance of rust generated on the surface of the produced soft magnetic powder was observed. The deposited phase of the produced soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase. Moreover, the produced soft magnetic powder was heat-treated in an argon atmosphere at the heat treatment temperature shown in Table 3 in an argon atmosphere. The saturation magnetic flux density Bs of the heat-treated soft magnetic powder was measured with a vibrating sample magnetometer (VSM). Table 3 shows the results of measurement and evaluation of the produced soft magnetic powder.
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
　表３に示されるように、Ｃｒを含まない比較例９においては、表面に錆の発生が確認された。一方、実施例１３～２５においては、表面に錆の発生が概ね認められなかった。飽和磁束密度Ｂｓについては、実施例１３～２５においては１．３４～１．７４Ｔであった。 As shown in Table 3, in Comparative Example 9 containing no Cr, generation of rust was confirmed on the surface. On the other hand, in Examples 13 to 25, almost no rust was observed on the surface. The saturation magnetic flux density Bs was 1.34 to 1.74 T in Examples 13 to 25.
　実施例１３～２５及び比較例９、１０の軟磁性粉末から圧粉磁芯を作製した。詳しくは、上述の方法で作製された軟磁性粉末を、２質量％のシリコーン樹脂を使用して造粒し、外径１３ｍｍ且つ内径８ｍｍの金型を使用して１０ｔｏｎ／ｃｍ２の成型圧力によって成型し硬化処理を施した。その後、電気炉にてアルゴン雰囲気中で表３に示す熱処理温度にて熱処理を行い、圧粉磁芯を作製した。得られた圧粉磁芯について、交流ＢＨアナライザーを使用して２０ｋＨｚ－１００ｍＴのコアロスを測定した。また、得られた圧粉磁芯について、６０℃－９０％ＲＨにおける恒温恒湿試験を実施し、外観観察にて腐食状況を確認した。作製された圧粉磁芯の測定及び評価の結果を表４に示す。 Powder magnetic cores were produced from the soft magnetic powders of Examples 13 to 25 and Comparative Examples 9 and 10. Specifically, the soft magnetic powder produced by the above-described method is granulated using 2% by mass of silicone resin, and a mold having an outer diameter of 13 mm and an inner diameter of 8 mm is used with a molding pressure of 10 ton / cm 2 . Molded and cured. Thereafter, heat treatment was performed in an electric furnace in an argon atmosphere at a heat treatment temperature shown in Table 3 to produce a dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. The obtained powder magnetic core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. Table 4 shows the results of measurement and evaluation of the produced dust core.
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
　表４に示されるように、比較例９、１０においては、コアロスが２９０～６６０ｋＷ／ｍ３であった。一方、実施例１３～２５においては、コアロスが７５～４２０ｋＷ／ｍ３であった。また、恒温恒湿試験においては、比較例９、比較例１０及び実施例１３において腐食が確認されたが、実施例１４～２５の全てにおいて腐食は概ね確認されなかった。 As shown in Table 4, in Comparative Examples 9 and 10, the core loss was 290 to 660 kW / m 3 . On the other hand, in Examples 13 to 25, the core loss was 75 to 420 kW / m 3 . In the constant temperature and humidity test, corrosion was confirmed in Comparative Example 9, Comparative Example 10 and Example 13, but in all of Examples 14 to 25, corrosion was generally not confirmed.
　上記の測定及び評価の結果において、比較例９と実施例１３との比較から、Ｃｒをわずかに添加した場合においても、軟磁性粉末における非晶質相の割合が著しく向上し、防錆の効果も発揮されることが理解される。軟磁性粉末中のＣｒの割合は、実施例２１と実施例２２との比較から、３ａｔ％以下が好ましいことが理解される。軟磁性粉末中のＣｒの割合は、実施例１８と実施例１９との比較から、１．８ａｔ％以下がより好ましく、１．５ａｔ％以下が更に好ましいことが理解される。軟磁性粉末中のＣｒの割合は、実施例１７と実施例１８とを飽和磁束密度Ｂｓの観点から比較すると、１ａｔ％以下がより好ましいことが理解される。また、軟磁性粉末中のＣｒの割合は、実施例１３と実施例１４との比較から、０．１ａｔ％以上が好ましいことが理解される。軟磁性粉末中のＣｒの割合は、実施例１４と実施例１５とをコアロスの観点から比較すると、０．５ａｔ％以上がより好ましいことが理解される。 As a result of the above measurement and evaluation, the comparison between Comparative Example 9 and Example 13 shows that even when Cr is added slightly, the proportion of the amorphous phase in the soft magnetic powder is remarkably improved, and the effect of rust prevention. It is understood that From the comparison between Example 21 and Example 22, it is understood that the Cr content in the soft magnetic powder is preferably 3 at% or less. From the comparison between Example 18 and Example 19, it is understood that the Cr ratio in the soft magnetic powder is more preferably 1.8 at% or less, and further preferably 1.5 at% or less. When the ratio of Cr in the soft magnetic powder is compared between Example 17 and Example 18 from the viewpoint of the saturation magnetic flux density Bs, it is understood that 1 at% or less is more preferable. Moreover, it is understood from the comparison between Example 13 and Example 14 that the Cr content in the soft magnetic powder is preferably 0.1 at% or more. It is understood that the ratio of Cr in the soft magnetic powder is more preferably 0.5 at% or more when Example 14 and Example 15 are compared from the viewpoint of core loss.
　また上記の測定及び評価の結果において、比較例１０と実施例２４、２５との比較から、Ｃｕの含有量の増大と共に防錆性が増大していることが理解される。軟磁性粉末中のＣｕの割合は、実施例１５と実施例２３とを非晶質相及びコアロスの観点から比較すると、０．７ａｔ％未満が好ましいことが理解される。軟磁性粉末中のＣｕの割合は、実施例１５と実施例１６とを非晶質相及びコアロスの観点から比較すると、０．６５ａｔ％以下がより好ましいことが理解される。また、軟磁性粉末中のＣｕの割合は、比較例１０と実施例２５との比較から、０．４ａｔ％以上が好ましいことが理解される。軟磁性粉末中のＣｕの割合は、実施例２４と実施例２５との比較から、０．５ａｔ％以上がより好ましいことが理解される。 Also, in the results of the above measurement and evaluation, it is understood from the comparison between Comparative Example 10 and Examples 24 and 25 that the rust preventive property increases as the Cu content increases. It is understood that the proportion of Cu in the soft magnetic powder is preferably less than 0.7 at% when comparing Example 15 and Example 23 from the viewpoint of the amorphous phase and the core loss. It is understood that the ratio of Cu in the soft magnetic powder is more preferably 0.65 at% or less when Example 15 and Example 16 are compared from the viewpoint of the amorphous phase and the core loss. Further, it is understood from the comparison between Comparative Example 10 and Example 25 that the Cu ratio in the soft magnetic powder is preferably 0.4 at% or more. From the comparison between Example 24 and Example 25, it is understood that the ratio of Cu in the soft magnetic powder is more preferably 0.5 at% or more.
　（実施例２６～３６）
　下記の表５に記載の実施例２６～３６の軟磁性粉末の原料として、工業純鉄、フェロシリコン、フェロリン、フェロボロン、電解銅、フェロクロム、フェロカーボン、ニオブ、モリブデン、Ｃｏ、Ｎｉ、錫、亜鉛、Ｍｎを準備した。原料を表５に記載の実施例２６～３６の合金組成となるように秤量し、アルゴン雰囲気中で高周波溶解によって溶解して合金溶湯を作製した。次に、作製された合金溶湯をガスアトマイズした後、冷却水により急冷して、平均粒径５０μｍの軟磁性粉末を作製した。作製された軟磁性粉末の表面に生じた錆の状態を外観観察した。作製された軟磁性粉末の析出相をＸ線回析（ＸＲＤ：X‐ray diffraction）によって評価して非晶質相の割合を算出した。また、作製された軟磁性粉末を、電気炉にてアルゴン雰囲気中で表５に示す熱処理温度にて熱処理を行った。熱処理された軟磁性粉末について振動試料型磁力計（ＶＳＭ）で飽和磁束密度Ｂｓを測定した。作製された軟磁性粉末の測定及び評価の結果を表５に示す。 (Examples 26 to 36)
As raw materials for the soft magnetic powders of Examples 26 to 36 shown in Table 5 below, industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, ferrochrome, ferrocarbon, niobium, molybdenum, Co, Ni, tin, zinc , Mn was prepared. The raw materials were weighed so as to have the alloy compositions of Examples 26 to 36 shown in Table 5, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 μm. The appearance of rust generated on the surface of the produced soft magnetic powder was observed. The deposited phase of the produced soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase. Moreover, the produced soft magnetic powder was heat-treated in an argon atmosphere in an argon atmosphere at a heat treatment temperature shown in Table 5. The saturation magnetic flux density Bs of the heat-treated soft magnetic powder was measured with a vibrating sample magnetometer (VSM). Table 5 shows the results of measurement and evaluation of the produced soft magnetic powder.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005
　実施例２６～３６においては、Ｍ元素（Ｃо、Ｎｉ、Ｃｕ、Ｚｎ、Ｍｎ）の添加や、Ｎｂ、Ｍｏ、Ｓｎ、ＣなどのＦｅへの置換が行われている。表５に示されるように、実施例２６～３６においては、表面に錆の発生は認められず、飽和磁束密度Ｂｓについては１．５８～１．７２Ｔであった。実施例２６、２９及び３１の比較から、ＣをＦｅと置換した場合、Ｆｅの割合が高い場合においても非晶質の割合を高く維持できることが理解できる。また、実施例３２から、Ｃｏを添加すると飽和磁束密度Ｂｓが向上することが理解される。 In Examples 26 to 36, addition of M element (Cо, Ni, Cu, Zn, Mn) and substitution of Fe with Nb, Mo, Sn, C, etc. are performed. As shown in Table 5, in Examples 26 to 36, no rust was observed on the surface, and the saturation magnetic flux density Bs was 1.58 to 1.72 T. From the comparison of Examples 26, 29 and 31, it can be understood that when C is replaced with Fe, the amorphous ratio can be kept high even when the ratio of Fe is high. Further, from Example 32, it is understood that the saturation magnetic flux density Bs is improved when Co is added.
　実施例２６～３６の軟磁性粉末から圧粉磁芯を作製した。詳しくは、上述の方法で作製された軟磁性粉末を、２質量％のシリコーン樹脂を使用して造粒し、外径１３ｍｍ且つ内径８ｍｍの金型を使用して１０ｔｏｎ／ｃｍ２の成型圧力によって成型し硬化処理を施した。その後、電気炉にてアルゴン雰囲気中で表５に示す熱処理温度にて熱処理を行い、圧粉磁芯を作製した。得られた圧粉磁芯について、交流ＢＨアナライザーを使用して２０ｋＨｚ－１００ｍＴのコアロスを測定した。また、得られた圧粉磁芯について、６０℃－９０％ＲＨにおける恒温恒湿試験を実施し、外観観察にて腐食状況を確認した。作製された圧粉磁芯の測定及び評価の結果を表６に示す。 A dust core was prepared from the soft magnetic powders of Examples 26 to 36. Specifically, the soft magnetic powder produced by the method described above, and granulated using a 2 wt% silicone resin, the molding pressure of 10ton / cm 2 using a mold having an outer diameter of 13mm and inner diameter of 8mm Molded and cured. Then, it heat-processed with the heat processing temperature shown in Table 5 in argon atmosphere with the electric furnace, and produced the dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. The obtained powder magnetic core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. Table 6 shows the results of measurement and evaluation of the produced dust core.
Figure JPOXMLDOC01-appb-T000006
Figure JPOXMLDOC01-appb-T000006
　表６に示されるように、実施例２６～３６においては、コアロスが７０～１３０ｋＷ/ｍ３と良好な結果であった。また、恒温恒湿試験においては、実施例２６～３６の全てにおいて腐食は概ね確認されなかった。 As shown in Table 6, in Examples 26 to 36, the core loss was a good result of 70 to 130 kW / m 3. In the constant temperature and humidity test, no corrosion was observed in all of Examples 26 to 36.
　実施例２６～２９、３１、３５に係る上記測定及び評価の結果から、Ｎｂ、Ｍｏ、Ｓｎ、ＣをＦｅと３ａｔ％以下の範囲で置換しても良好な軟磁気特性や防食性を示すことが理解された。特に、実施例２７、２８のようにＮｂやＭｏへの置換によりコアロスの低減や防錆効果の向上が図られることが理解される。 From the results of the above measurements and evaluations relating to Examples 26 to 29, 31, and 35, good soft magnetic properties and anticorrosion properties are exhibited even when Nb, Mo, Sn, and C are replaced with Fe in a range of 3 at% or less. Was understood. In particular, it is understood that the replacement with Nb or Mo as in Examples 27 and 28 can reduce the core loss and improve the rust prevention effect.
　実施例３２～３４及び実施例３６に係る上記測定及び評価の結果から、Ｃｕ以外のＭ元素を添加しても良好な軟磁気特性や防食性を示すことが理解された。特に、実施例３３、３４のようにＮｉやＺｎを添加すると、防錆効果の向上が図られることが理解される。 From the results of the above measurements and evaluations relating to Examples 32 to 34 and Example 36, it was understood that good soft magnetic properties and anticorrosion properties were exhibited even when M elements other than Cu were added. In particular, it is understood that when Ni or Zn is added as in Examples 33 and 34, the rust prevention effect is improved.
　（実施例３７～４５、比較例１１）
　下記の表７に記載の実施例３７～４５、比較例１１の軟磁性粉末の原料として、工業純鉄、フェロシリコン、フェロリン、フェロボロン、電解銅、フェロクロムを準備した。原料を表７に記載の実施例３７～４５、比較例１１の合金組成となるように秤量し、アルゴン雰囲気中で高周波溶解によって溶解して合金溶湯を作製した。次に、作製された合金溶湯をガスアトマイズした後、冷却水により急冷して、平均粒径５０μｍの軟磁性粉末を作製した。作製された軟磁性粉末を、２質量％のシリコーン樹脂を使用して造粒し、外径１３ｍｍ且つ内径８ｍｍの金型を使用して１０ｔｏｎ／ｃｍ２の成型圧力によって成型し硬化処理を施した。その後、電気炉にてアルゴン雰囲気中で表７に示す熱処理温度にて熱処理を行い、圧粉磁芯を作製した。得られた圧粉磁芯について、交流ＢＨアナライザーを使用して２０ｋＨｚ－１００ｍＴのコアロスを測定した。加えて、得られた圧粉磁芯の表面をＸＲＤ測定してＷＰＰＤ法で解析することにより、圧粉磁芯に含まれる軟磁性粉末中のαＦｅのナノ結晶の平均粒径及び結晶化度、並びにαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度を、夫々算出した。作製された圧粉磁芯の測定及び評価の結果を表７に示す。なお、表７中において、αＦｅのナノ結晶の平均粒径、αＦｅのナノ結晶の結晶化度及びαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度を、夫々、αＦｅ結晶粒径、αＦｅ結晶化度及び化合物相結晶化度と表記している。 (Examples 37 to 45, Comparative Example 11)
Industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, and ferrochrome were prepared as raw materials for the soft magnetic powders of Examples 37 to 45 and Comparative Example 11 shown in Table 7 below. The raw materials were weighed so as to have the alloy compositions of Examples 37 to 45 and Comparative Example 11 shown in Table 7, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 μm. The produced soft magnetic powder was granulated using 2% by mass of a silicone resin, and molded by a molding pressure of 10 ton / cm 2 using a mold having an outer diameter of 13 mm and an inner diameter of 8 mm, followed by a curing treatment. . Thereafter, heat treatment was performed in an electric furnace in an argon atmosphere at a heat treatment temperature shown in Table 7 to produce a dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. In addition, by measuring the surface of the obtained dust core by XRD and analyzing by the WPPD method, the average particle diameter and crystallinity of the αFe nanocrystals in the soft magnetic powder contained in the dust core, In addition, the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystal was calculated. Table 7 shows the results of measurement and evaluation of the produced dust core. In Table 7, the average particle diameter of the αFe nanocrystals, the crystallinity of the αFe nanocrystals, and the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystals are expressed as αFe crystal particle diameter, αFe, respectively. It is expressed as crystallinity and compound phase crystallinity.
Figure JPOXMLDOC01-appb-T000007
Figure JPOXMLDOC01-appb-T000007
　実施例３７～４２は、互いに同じ元素組成を有しているが、熱処理条件のみが異なっている。また、実施例４３～４５も、互いに同じ元素組成を有しているが、熱処理条件のみが異なっている。表７に示されるように、同じ元素組成を有する軟磁性粉末から作製された圧粉磁芯であっても、熱処理条件の相違により、コアロス、αＦｅのナノ結晶の結晶粒径及び結晶化度、並びにαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度が、大きく相違することが理解される。 Examples 37 to 42 have the same elemental composition, but only the heat treatment conditions are different. Examples 43 to 45 also have the same elemental composition, but only the heat treatment conditions are different. As shown in Table 7, even in a dust core made of soft magnetic powder having the same elemental composition, due to the difference in heat treatment conditions, the core loss, the crystal grain size and crystallinity of αFe nanocrystals, In addition, it is understood that the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystal is greatly different.
　表７から、実施例３８～４１、４４、４５のように、熱処理を適切な温度及び時間で実施することにより、αＦｅのナノ結晶の結晶粒径の低減及び結晶化度の増大、並びにαＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度の低減が図られ、圧粉磁芯のコアロスの低減が図られることが理解される。 From Table 7, by performing the heat treatment at an appropriate temperature and time as in Examples 38 to 41, 44, 45, the crystal grain size of the αFe nanocrystals was reduced and the crystallinity was increased. It is understood that the crystallinity of the compound phase other than the bcc phase in the nanocrystal is reduced, and the core loss of the dust core is reduced.
　比較例１１及び実施例４３を、コアロス及びαＦｅのナノ結晶の結晶粒径の観点から対比すると、比較例１１のようにαＦｅのナノ結晶の結晶粒径が粗大化した場合、コアロスが増大することが分かる。従って、αＦｅのナノ結晶の結晶粒径は５０ｎｍ以下が好ましいことが理解される。 Comparing Comparative Example 11 and Example 43 from the viewpoint of the core loss and the crystal grain size of αFe nanocrystals, the core loss increases when the crystal grain size of αFe nanocrystals becomes coarse as in Comparative Example 11. I understand. Therefore, it is understood that the crystal grain size of the αFe nanocrystal is preferably 50 nm or less.
　また、実施例３７及び実施例４３を、コアロス及びαＦｅのナノ結晶の結晶化度の観点から対比すると、実施例４３のようにαＦｅのナノ結晶の結晶化度が低い場合、磁歪の低減が十分図られず、コアロスが増大することが分かる。従って、αＦｅのナノ結晶の結晶化度は３５％以上が好ましいことが理解される。 Further, when Example 37 and Example 43 are compared from the viewpoint of the crystallinity of the core loss and the αFe nanocrystal, when the crystallinity of the αFe nanocrystal is low as in Example 43, the magnetostriction is sufficiently reduced. It can be seen that the core loss increases. Therefore, it is understood that the crystallinity of αFe nanocrystals is preferably 35% or more.
　更に、実施例４０、４１、４２、４５を参照すると、αＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度の増大と共に、コアロスが増大することが理解される。従って、実施例４０、４１、４５を参照して、αＦｅのナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度は、７％以下が好ましく、５％以下がより好ましく、３％以下が更に好ましいことが理解される。 Furthermore, referring to Examples 40, 41, 42, and 45, it is understood that the core loss increases as the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystal increases. Therefore, referring to Examples 40, 41, and 45, the crystallinity of the compound phase other than the bcc phase in the αFe nanocrystal is preferably 7% or less, more preferably 5% or less, and still more preferably 3% or less. It is understood.
　（実施例４６～６６）
　下記の表８に記載の実施例４６～６６の軟磁性粉末の原料として、工業純鉄、フェロシリコン、フェロリン、フェロボロン、電解銅、フェロクロム及び、Ｍｎ、Ａｌ、Ｔｉ、ＦｅＳを準備した。原料を表８に記載の実施例４６～６６の合金組成となるように秤量し、アルゴン雰囲気中で高周波溶解によって溶解して合金溶湯を作製した。次に、作製された合金溶湯をガスアトマイズした後、冷却水により急冷して、平均粒径５０μｍの軟磁性粉末を作製した。 (Examples 46 to 66)
Industrial pure iron, ferrosilicon, ferroline, ferroboron, electrolytic copper, ferrochrome, and Mn, Al, Ti, FeS were prepared as raw materials for the soft magnetic powders of Examples 46 to 66 shown in Table 8 below. The raw materials were weighed so as to have the alloy compositions of Examples 46 to 66 shown in Table 8, and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the produced molten alloy was gas atomized and then quenched with cooling water to produce a soft magnetic powder having an average particle size of 50 μm.
Figure JPOXMLDOC01-appb-T000008
Figure JPOXMLDOC01-appb-T000008
　実施例４６～６６の軟磁性粉末の表面に生じた錆の状態を外観観察した。軟磁性粉末の析出相をＸ線回析（ＸＲＤ：X‐ray diffraction）によって評価して非晶質相の割合を算出した。また、作製された軟磁性粉末を、電気炉にてアルゴン雰囲気中で表９に示す熱処理温度にて熱処理を行い、熱処理された軟磁性粉末について振動試料型磁力計（ＶＳＭ）で飽和磁束密度Ｂｓを測定した。作製された軟磁性粉末の測定及び評価の結果を表９に示す。 The appearance of rust produced on the surfaces of the soft magnetic powders of Examples 46 to 66 was observed. The precipitated phase of the soft magnetic powder was evaluated by X-ray diffraction (XRD) to calculate the proportion of the amorphous phase. Further, the produced soft magnetic powder was heat-treated in an electric furnace in an argon atmosphere at the heat treatment temperature shown in Table 9, and the heat-treated soft magnetic powder was subjected to a saturation magnetic flux density Bs with a vibrating sample magnetometer (VSM). Was measured. Table 9 shows the results of measurement and evaluation of the produced soft magnetic powder.
　また、実施例４６～６６の軟磁性粉末から圧粉磁芯を作製した。詳しくは、上述の方法で作製された軟磁性粉末を、２質量％のシリコーン樹脂を使用して造粒し、外径１３ｍｍ且つ内径８ｍｍの金型を使用して１０ｔｏｎ／ｃｍ２の成型圧力によって成型し硬化処理を施した。その後、電気炉にてアルゴン雰囲気中で表９に示す熱処理温度にて熱処理を行い、圧粉磁芯を作製した。得られた圧粉磁芯について、交流ＢＨアナライザーを使用して２０ｋＨｚ－１００ｍＴのコアロスを測定した。また、得られた圧粉磁芯について、６０℃－９０％ＲＨにおける恒温恒湿試験を実施し、外観観察にて腐食状況を確認した。作製された圧粉磁芯の測定及び評価の結果を表９に示す。 Further, dust cores were produced from the soft magnetic powders of Examples 46 to 66. Specifically, the soft magnetic powder produced by the above-described method is granulated using 2% by mass of silicone resin, and a mold having an outer diameter of 13 mm and an inner diameter of 8 mm is used with a molding pressure of 10 ton / cm 2 . Molded and cured. Thereafter, heat treatment was performed at a heat treatment temperature shown in Table 9 in an argon atmosphere in an electric furnace to produce a dust core. About the obtained powder magnetic core, the core loss of 20 kHz-100 mT was measured using the AC BH analyzer. The obtained powder magnetic core was subjected to a constant temperature and humidity test at 60 ° C. to 90% RH, and the corrosion state was confirmed by appearance observation. Table 9 shows the results of measurement and evaluation of the produced dust core.
Figure JPOXMLDOC01-appb-T000009
Figure JPOXMLDOC01-appb-T000009
　実施例４６～６６は、Ａｌ、Ｔｉ、Ｓ、Ｎ、Ｏを微量元素として様々な含有量で含有している。また、実施例４６～６２は、同一のＦｅ、Ｓｉ、Ｂ、Ｐ、Ｃｕ及びＣｒの元素組成を有している。表９から、非晶質相の割合については、実施例４６、４８、４９、５１～６６について、９２％以上と高い値を示すことが理解される。また、表９から、飽和磁束密度Ｂｓについては、実施例４６～５２及び５４～６６について、１．５８Ｔ以上と良好な値を示すことが理解される。更に、表９から、コアロスについては、実施例４６、４８、４９、５１～５８、６０～６６について、２２０ｋＷ／ｍ３以下と良好な値を示すことが理解される。一方、微量元素のうち、Ａｌ、Ｔｉ、Ｓ、Ｏの含有量が多い実施例４７、実施例５０、実施例５３及び実施例５９の飽和磁束密度Ｂｓは、微量元素の含有量が少ない表９の残りの実施例と比べて低い。しかしながら、実施例４７、実施例５０、実施例５３及び実施例５９の飽和磁束密度Ｂｓは、１．５４Ｔ以上の値を示すことが理解される。 Examples 46 to 66 contain Al, Ti, S, N, and O as trace elements in various contents. Examples 46 to 62 have the same elemental composition of Fe, Si, B, P, Cu and Cr. From Table 9, it is understood that the ratio of the amorphous phase shows a high value of 92% or more for Examples 46, 48, 49, and 51 to 66. Also, from Table 9, it is understood that the saturation magnetic flux density Bs shows a good value of 1.58 T or more for Examples 46 to 52 and 54 to 66. Furthermore, it can be seen from Table 9 that the core loss shows a good value of 220 kW / m 3 or less for Examples 46, 48, 49, 51 to 58, and 60 to 66. On the other hand, among the trace elements, the saturation magnetic flux density Bs of Examples 47, 50, 53, and 59 having a large content of Al, Ti, S, and O is low in the trace element content. Compared to the rest of the examples. However, it is understood that the saturation magnetic flux density Bs of Example 47, Example 50, Example 53, and Example 59 shows a value of 1.54 T or more.
　実施例４６及び実施例４７～４９を参照すると、Ａｌの含有量の増大と共に、非晶質の割合及び飽和磁束密度Ｂｓが低下し、且つ、コアロスが増大することが理解される。即ち、Ａｌの含有量は、非晶質の割合、飽和磁束密度Ｂｓ及びコアロスの観点から、０．０５質量％以下であることが好ましく、またコアロスの低減の観点から０．００５質量％以下であることがより好ましいことが理解される。 Referring to Example 46 and Examples 47 to 49, it can be understood that as the Al content increases, the amorphous ratio and the saturation magnetic flux density Bs decrease, and the core loss increases. That is, the content of Al is preferably 0.05% by mass or less from the viewpoint of amorphous ratio, saturation magnetic flux density Bs and core loss, and 0.005% by mass or less from the viewpoint of core loss reduction. It is understood that there is more preferred.
　実施例４６及び実施例５０～５２を参照すると、Ｔｉの含有量の増大と共に、非晶質の割合及び飽和磁束密度Ｂｓが低下し、且つ、コアロスが増大することが理解される。即ち、Ｔｉの含有量は、非晶質の割合、飽和磁束密度Ｂｓ及びコアロスの観点から、０．０５質量％以下であることが好ましく、またコアロスの低減の観点から０．００５質量％以下であることがより好ましいことが理解される。 Referring to Example 46 and Examples 50 to 52, it is understood that as the Ti content increases, the amorphous ratio and the saturation magnetic flux density Bs decrease, and the core loss increases. That is, the content of Ti is preferably 0.05% by mass or less from the viewpoint of amorphous ratio, saturation magnetic flux density Bs and core loss, and 0.005% by mass or less from the viewpoint of core loss reduction. It is understood that there is more preferred.
　実施例４６及び実施例５３～５５を参照すると、Ｓの含有量の増大と共に、非晶質の割合及び飽和磁束密度Ｂｓが低下することが理解される。Ｓの含有量は、非晶質の割合及び飽和磁束密度Ｂｓの観点から、０．５質量％以下であることが好ましく、また、防食性の観点から０．０５質量％以下であることがより好ましいことが理解される。 Referring to Example 46 and Examples 53 to 55, it is understood that the amorphous ratio and the saturation magnetic flux density Bs decrease as the S content increases. The content of S is preferably 0.5% by mass or less from the viewpoint of the amorphous ratio and the saturation magnetic flux density Bs, and more preferably 0.05% by mass or less from the viewpoint of corrosion resistance. It is understood that it is preferable.
　実施例４６及び実施例５６～５８を参照すると、Ｎの含有量の増大と共に、非晶質の割合が低下し、且つ、コアロスが増大することが理解される。即ち、Ｎの含有量は、非晶質の割合及びコアロスの観点から、０．０１質量％以下であることが好ましく、０．００２質量％以下であることがより好ましいことが理解される。 Referring to Example 46 and Examples 56 to 58, it is understood that as the N content increases, the amorphous ratio decreases and the core loss increases. That is, it is understood that the N content is preferably 0.01% by mass or less and more preferably 0.002% by mass or less from the viewpoint of the amorphous ratio and the core loss.
　実施例５９、実施例６０及び実施例６１を参照すると、Ｏの含有量の増大と共に耐食性が低下することが理解される。即ち、Ｏの含有量は、耐食性の観点から、１質量％以下であることが好ましく、０．３質量％以下であることがより好ましいことが理解される。 Referring to Example 59, Example 60, and Example 61, it is understood that the corrosion resistance decreases as the O content increases. That is, it is understood that the content of O is preferably 1% by mass or less and more preferably 0.3% by mass or less from the viewpoint of corrosion resistance.
　（インダクタ）
　本実施の形態の軟磁性粉末を用いてインダクタを作製し、作製されたインダクタの直流重畳特性の評価を行った。インダクタの製作方法を以下に詳述する。 (Inductor)
An inductor was fabricated using the soft magnetic powder of the present embodiment, and the DC superposition characteristics of the fabricated inductor were evaluated. The method for manufacturing the inductor will be described in detail below.
　まず、軟磁性粉末の原料として、工業純鉄、フェロシリコン、フェロリン、フェロボロン、及び電解銅を準備した。原料をＦｅ８２．１Ｓｉ２．９Ｂ５Ｐ８．８Ｃｕ０．６５Ｃｒ０．５５の合金組成となるように秤量し、アルゴン雰囲気中で高周波溶解によって溶解して合金溶湯を作製した。次に、作製された合金溶湯をガスアトマイズした後、冷却水により急冷して、平均粒径５０μｍの軟磁性粉末Ａを作製した。また、作製された合金溶湯を水アトマイズにより、平均粒径１０μｍの軟磁性粉末Ｂを作製した。作製された２種類の軟磁性粉末Ａ及びＢを、Ａ：Ｂ＝８：２の質量割合で混合したうえで、結合剤としてのシリコーン樹脂を添加してさらに混合し、この軟磁性粉末Ａ，Ｂと結合剤との混合物を造粒して造粒粉末を作製した。このとき、結合剤であるシリコーン樹脂は、軟磁性粉末Ａと軟磁性粉末Ｂの合量に対して２質量％となるように添加した。 First, industrial pure iron, ferrosilicon, ferroline, ferroboron, and electrolytic copper were prepared as raw materials for the soft magnetic powder. The raw materials were weighed so as to have an alloy composition of Fe 82.1 Si 2.9 B 5 P 8.8 Cu 0.65 Cr 0.55 and melted by high frequency melting in an argon atmosphere to prepare a molten alloy. Next, the prepared molten alloy was gas atomized and then quenched with cooling water to prepare soft magnetic powder A having an average particle size of 50 μm. Further, soft magnetic powder B having an average particle diameter of 10 μm was produced by water atomization of the produced molten alloy. The two types of soft magnetic powders A and B thus prepared were mixed at a mass ratio of A: B = 8: 2, and a silicone resin as a binder was added and further mixed. A mixture of B and a binder was granulated to produce a granulated powder. At this time, the silicone resin as a binder was added so as to be 2% by mass with respect to the total amount of the soft magnetic powder A and the soft magnetic powder B.
　次に、コイルとして、図１に示すコイル１２０を用意した。このコイル１２０は、平角導線１２１をエッジワイズ巻きしたものであり、巻数は３．５ターンとなっている。ここで、平角導線１２１は、断面形状が２．０ｍｍ×０．６ｍｍの長方形であり、表面に厚さ２０μｍのポリアミドイミドからなる絶縁層を有している。また、コイル１２０は、両端に表面実装用端子１２２を有している。このコイル１２０を予め金型内に配置した状態で、金型のキャビティに上述の造粒粉末を充填し、５ｔｏｎ／ｃｍ２の成型圧力によって、造粒粉末とコイル１２０とを一体で加圧成型して硬化処理を施し、成型体を製造した。この成型体を、電気炉にてアルゴン雰囲気中で４００℃、３０分間熱処理を行い、圧粉磁芯１１０の内部にコイル１２０が埋め込まれた、実施例のインダクタ１００を作製した。 Next, the coil 120 shown in FIG. 1 was prepared as a coil. This coil 120 is obtained by winding a flat conducting wire 121 edgewise, and the number of turns is 3.5 turns. Here, the flat conducting wire 121 is a rectangle having a cross-sectional shape of 2.0 mm × 0.6 mm, and has an insulating layer made of polyamideimide having a thickness of 20 μm on the surface. The coil 120 has surface mounting terminals 122 at both ends. With the coil 120 placed in the mold in advance, the above-mentioned granulated powder is filled in the mold cavity, and the granulated powder and the coil 120 are integrally pressure-molded by a molding pressure of 5 ton / cm 2. Then, a curing treatment was performed to produce a molded body. The molded body was heat-treated in an electric furnace in an argon atmosphere at 400 ° C. for 30 minutes, and the inductor 100 of the example in which the coil 120 was embedded inside the dust core 110 was produced.
　また、比較例のインダクタ１００Ａとして、軟磁性粉末Ａ及びＢの代わりにＦｅ-Ｓｉ-Ｃｒ粉末を用いて、上述の実施例のインダクタ１００と同様の製造方法により、圧粉磁芯１１０Ａの内部にコイル１２０が埋め込まれたインダクタ１００Ａを作製した。なお、比較例のインダクタ１００Ａのコイル１２０は、実施例のインダクタ１００のコイル１２０と同様の構造を有しているため、詳細な説明は省略する。 In addition, as the inductor 100A of the comparative example, Fe—Si—Cr powder is used instead of the soft magnetic powders A and B, and the same manufacturing method as that of the inductor 100 of the above-described embodiment is used. An inductor 100A in which the coil 120 was embedded was manufactured. Since the coil 120 of the inductor 100A of the comparative example has the same structure as the coil 120 of the inductor 100 of the embodiment, detailed description thereof is omitted.
　図１及び図２に示されるように、実施例のインダクタ１００は、圧粉磁芯１１０の内部にコイル１２０が埋め込まれた、一体成型型のインダクタ１００となっている。また、コイル１２０の表面実装用端子１２２は、圧粉磁芯１１０の外部に引き出されている。 As shown in FIGS. 1 and 2, the inductor 100 according to the embodiment is an integrally molded inductor 100 in which a coil 120 is embedded in a dust core 110. Further, the surface mounting terminal 122 of the coil 120 is drawn to the outside of the dust core 110.
　また、図３に示されるように、比較例のインダクタ１００Ａは、実施例のインダクタ１００と同様に、圧粉磁芯１１０Ａの内部にコイル１２０が埋め込まれた、一体成型型のインダクタ１００Ａとなっており、コイル１２０の表面実装用端子１２２は、圧粉磁芯１１０Ａの外部に引き出されている。 Also, as shown in FIG. 3, the inductor 100A of the comparative example is an integrally molded inductor 100A in which the coil 120 is embedded in the dust core 110A, like the inductor 100 of the embodiment. The surface mounting terminal 122 of the coil 120 is drawn out of the dust core 110A.
　図４は、実施例及び比較例のインダクタ１００，１００Ａの直流重畳特性を示している。図４から、実施例のインダクタ１００は、比較例のインダクタ１００Ａと比較して、印加する電流Ｉの増大に伴うインダクタンスＬの低下の割合が小さいことが理解される。即ち、実施例のインダクタ１００は、比較例のインダクタ１００Ａと比較して、優れた直流重畳特性を示すことが理解される。 FIG. 4 shows the DC superposition characteristics of the inductors 100 and 100A of the example and the comparative example. From FIG. 4, it is understood that the inductor 100 of the example has a smaller rate of decrease of the inductance L due to the increase of the applied current I than the inductor 100A of the comparative example. That is, it can be understood that the inductor 100 of the example exhibits superior DC superposition characteristics as compared with the inductor 100A of the comparative example.
　本発明は２０１７年２月１６日に日本国特許庁に提出された日本特許出願第２０１７－２７１６２号及び２０１７年１０月２５日に日本国特許庁に提出された日本特許出願第２０１７－２０６６０８号に基づいており、その内容は参照することにより本明細書の一部をなす。 The present invention relates to Japanese Patent Application No. 2017-27162 filed with the Japan Patent Office on February 16, 2017 and Japanese Patent Application No. 2017-206608 filed with the Japan Patent Office on October 25, 2017. The contents of which are incorporated herein by reference.
　本発明の最良の実施の形態について説明したが、当業者には明らかなように、本発明の精神を逸脱しない範囲で実施の形態を変形することが可能であり、そのような実施の形態は本発明の範囲に属するものである。
Although the best embodiment of the present invention has been described, it will be apparent to those skilled in the art that the embodiment can be modified without departing from the spirit of the present invention. It belongs to the scope of the present invention.
　１００，１００Ａ　　インダクタ
　１１０，１１０Ａ　　圧粉磁芯
　１２０　　コイル
　１２１　　平角導線
　１２２　　表面実装用端子 100, 100A Inductor 110, 110A Dust core 120 Coil 121 Flat conductor 122 Terminal for surface mounting

Claims (24)

  1. 　不可避不純物を除き組成式ＦｅａＳｉｂＢｃＰｄＣｒｅＭｆで表される軟磁性粉末であって、
    　Ｍは、Ｖ、Ｍｎ、Ｃｏ、Ｎｉ、Ｃｕ、Ｚｎから選ばれる１種以上の元素であり、
    　０ａｔ％≦ｂ≦６ａｔ％、４ａｔ％≦ｃ≦１０ａｔ％、５ａｔ％≦ｄ≦１２ａｔ％、０ａｔ％＜ｅ、０．４ａｔ％≦ｆ＜６ａｔ％、且つ、ａ＋ｂ＋ｃ＋ｄ＋ｅ＋ｆ＝１００ａｔ％である
    軟磁性粉末。     A soft magnetic powder represented by the composition formula Fe a Si b B c P d Cr e M f excluding inevitable impurities,
    M is one or more elements selected from V, Mn, Co, Ni, Cu, Zn,
    Soft magnetic powder with 0 at% ≦ b ≦ 6 at%, 4 at% ≦ c ≦ 10 at%, 5 at% ≦ d ≦ 12 at%, 0 at% <e, 0.4 at% ≦ f <6 at%, and a + b + c + d + e + f = 100 at% .
  2. 　請求項１記載の軟磁性粉末であって、
    　前記ＭはＣｕを含んでおり、
    　ＭｆはＣｕｇＭ´ｈで表され、
    　Ｍ´は、Ｖ、Ｍｎ、Ｃｏ、Ｎｉ、Ｚｎから選ばれる１種以上の元素であり、
    　７８ａｔ％≦ａ≦８５ａｔ％、ｅ≦３ａｔ％、０．４ａｔ％≦ｇ＜０．７ａｔ％、且つｆ＝ｇ＋ｈである
    軟磁性粉末。     The soft magnetic powder according to claim 1,
    M includes Cu,
    M f is represented by Cu g M ′ h ,
    M ′ is one or more elements selected from V, Mn, Co, Ni, and Zn,
    Soft magnetic powder with 78 at% ≦ a ≦ 85 at%, e ≦ 3 at%, 0.4 at% ≦ g <0.7 at%, and f = g + h.
  3. 　請求項２に記載の軟磁性粉末であって、
    　０．５ａｔ％≦ｇ≦０．６５ａｔ％である
    軟磁性粉末。     The soft magnetic powder according to claim 2,
    Soft magnetic powder satisfying 0.5 at% ≦ g ≦ 0.65 at%.
  4. 　請求項２又は請求項３記載の軟磁性粉末であって、
    　（０．２ｅ－０．１）ａｔ％≦ｇ≦（２ｅ＋０．５）ａｔ％、且つ（６－２ｅ）ａｔ％≦ｄ≦（２１－５ｅ）ａｔ％である
    軟磁性粉末。     The soft magnetic powder according to claim 2 or claim 3,
    Soft magnetic powder with (0.2e−0.1) at% ≦ g ≦ (2e + 0.5) at% and (6-2e) at% ≦ d ≦ (21-5e) at%.
  5. 　請求項１から請求項４までのいずれかに記載の軟磁性粉末であって、
    　５ａｔ％＜ｄ≦１０ａｔ％、且つ、０．１ａｔ％≦ｅである
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 4,
    Soft magnetic powder in which 5 at% <d ≦ 10 at% and 0.1 at% ≦ e.
  6. 　請求項１から請求項５までのいずれかに記載の軟磁性粉末であって、
    　６ａｔ％＜ｄ≦８ａｔ％、且つ、０．５ａｔ％≦ｅである
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 5,
    Soft magnetic powder in which 6 at% <d ≦ 8 at% and 0.5 at% ≦ e.
  7. 　請求項１から請求項５までのいずれかに記載の軟磁性粉末であって、
    　８ａｔ％＜ｄ≦１０ａｔ％である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 5,
    Soft magnetic powder with 8 at% <d ≦ 10 at%.
  8. 　請求項１から請求項７までのいずれかに記載の軟磁性粉末であって、
    　前記Ｆｅの３ａｔ％以下を、Ｎｂ、Ｚｒ、Ｈｆ、Ｍｏ、Ｔａ、Ｗ、Ａｇ、Ａｕ、Ｐｄ、Ｋ、Ｃａ、Ｍｇ、Ｓｎ、Ｔｉ、Ａｌ、Ｓ、Ｃ、Ｏ、Ｎ、Ｙ及び希土類元素から選ばれる１種類以上の元素で置換した
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 7,
    Fe of 3 at% or less of Fe, Nb, Zr, Hf, Mo, Ta, W, Ag, Au, Pd, K, Ca, Mg, Sn, Ti, Al, S, C, O, N, Y and rare earth elements Soft magnetic powder substituted with one or more elements selected from
  9. 　請求項１から請求項８までのいずれかに記載の軟磁性粉末であって、
    　７９ａｔ％≦ａ≦８３．５ａｔ％、且つ、ｅ≦１．８ａｔ％である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 8,
    Soft magnetic powder with 79 at% ≦ a ≦ 83.5 at% and e ≦ 1.8 at%.
  10. 　請求項１から請求項９までのいずれかに記載の軟磁性粉末であって、
    　８０．５ａｔ％≦ａである
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 9,
    Soft magnetic powder satisfying 80.5 at% ≦ a.
  11. 　請求項１から請求項１０までのいずれかに記載の軟磁性粉末であって、
    　ｅ≦１．５ａｔ％である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 10,
    Soft magnetic powder with e ≦ 1.5 at%.
  12. 　請求項１から請求項１１までのいずれかに記載の軟磁性粉末であって、
    　ｅ≦１．０ａｔ％である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 11,
    Soft magnetic powder with e ≦ 1.0 at%.
  13. 　請求項１から請求項１２までのいずれかに記載の軟磁性粉末であって、
    　０．１ａｔ％≦ｂである
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 12,
    Soft magnetic powder satisfying 0.1 at% ≦ b.
  14. 　請求項１から請求項１３までのいずれかに記載の軟磁性粉末であって、
    　Ａｌ、Ｔｉ、Ｓ、Ｎ、Ｏの含有量がＡｌ≦０．０５質量％、Ｔｉ≦０．０５質量％、Ｓ≦０．５質量％、Ｎ≦０．０１質量％、Ｏ≦１．０質量％である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 13,
    Al, Ti, S, N, O content is Al ≦ 0.05 mass%, Ti ≦ 0.05 mass%, S ≦ 0.5 mass%, N ≦ 0.01 mass%, O ≦ 1.0 Soft magnetic powder of mass%.
  15. 　請求項１から請求項１４までのいずれかに記載の軟磁性粉末であって、
    　Ａｌ、Ｔｉ、Ｓ、Ｎ、Ｏの含有量がＡｌ≦０．００５質量％、Ｔｉ≦０．００５質量％、Ｓ≦０．０５質量％、Ｎ≦０．００２質量％、Ｏ≦０．３質量％である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 14,
    Al, Ti, S, N, O content is Al ≦ 0.005 mass%, Ti ≦ 0.005 mass%, S ≦ 0.05 mass%, N ≦ 0.002 mass%, O ≦ 0.3 Soft magnetic powder of mass%.
  16. 　請求項１から請求項１５までのいずれかに記載の軟磁性粉末であって、
    　平均粒径が２００μｍ以下である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 15,
    Soft magnetic powder having an average particle size of 200 μm or less.
  17. 　請求項１から請求項１６までのいずれかに記載の軟磁性粉末であって、
    　非晶質相が９０％以上含まれている
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 16,
    Soft magnetic powder containing 90% or more amorphous phase.
  18. 　請求項１から請求項１７までのいずれかに記載の軟磁性粉末であって、
    　タップ密度が３．５ｇ／ｃｍ３以上である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 17,
    Soft magnetic powder having a tap density of 3.5 g / cm 3 or more.
  19. 　請求項１から請求項１８までのいずれかに記載の軟磁性粉末であって、
    　前記軟磁性粉末はナノ結晶を含有しており、
    　前記ナノ結晶の結晶化度は３５％以上である
    軟磁性粉末。     The soft magnetic powder according to any one of claims 1 to 18,
    The soft magnetic powder contains nanocrystals,
    A soft magnetic powder having a crystallinity of 35% or more of the nanocrystal.
  20. 　請求項１９記載の軟磁性粉末であって、
    　前記ナノ結晶におけるｂｃｃ相以外の化合物相の結晶化度が５％以下である
    軟磁性粉末。     The soft magnetic powder according to claim 19,
    The soft magnetic powder in which the crystallinity of the compound phase other than the bcc phase in the nanocrystal is 5% or less.
  21. 　請求項１から請求項２０までのいずれかに記載の軟磁性粉末を用いた圧粉磁芯。 A dust core using the soft magnetic powder according to any one of claims 1 to 20.
  22. 　請求項１から請求項２０までのいずれかに記載の軟磁性粉末と結合剤との混合物を製造する工程と、前記混合物を加圧成型して成型体を製造する工程と、前記成型体を熱処理する工程とを備える
    圧粉磁芯の製造方法。     A process for producing a mixture of the soft magnetic powder and the binder according to any one of claims 1 to 20, a process for producing a molded body by press molding the mixture, and heat-treating the molded body The manufacturing method of a dust core provided with the process to do.
  23. 　請求項１から請求項２０までのいずれかに記載の軟磁性粉末と結合剤との混合物を製造する工程と、前記混合物とコイルとを一体で加圧成型して成型体を製造する工程と、前記成型体を熱処理する工程とを備える
    インダクタの磁芯の製造方法。     A step of producing a mixture of the soft magnetic powder and the binder according to any one of claims 1 to 20, a step of producing a molded body by integrally pressing the mixture and the coil, and A method of manufacturing a magnetic core of an inductor comprising a step of heat-treating the molded body.
  24. 　請求項１から請求項２０までのいずれかに記載の軟磁性粉末を用いた磁性部品。 A magnetic part using the soft magnetic powder according to any one of claims 1 to 20.
PCT/JP2018/004021 2017-02-16 2018-02-06 Soft magnetic powder, dust magnetic core, magnetic part, and method for producing dust magnetic core WO2018150952A1 (en)

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